反応 #4146909
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-d3b0316260be4569bd738f32cbfc27bd表示可能な構造データがありません
CNCC(=O)OCC1=CC=CC=C1製品情報
benzyl 2-(methylamino)acetate (CAS 54384-05-3) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 7019103
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
10 反応 · 10 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-d3b0316260be4569bd738f32cbfc27bd反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-0ea382043e6642be93dc1fb60719a963反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-d3b0316260be4569bd738f32cbfc27bd反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-0ea382043e6642be93dc1fb60719a963反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-0ea382043e6642be93dc1fb60719a963反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-ccae603003f14fca9668b5a8da6d0d4d反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-ccae603003f14fca9668b5a8da6d0d4d反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Ac-Gly-OH a (4.10 g, 35.0 mmol), Sar-OBzl.PTSA b (11.71 g, 33.3 mmol), triethylamine (5.58 mL, 40.0 mmol), HOBt (1.35 g, 10 mmol) and DCC (8.25 g, 40.0 mmol) were stirred in 200 mL THF overnight. The mixture was filtered to discard DCU and removed THF in vacuum. The concentrated residue was dissolved in 100 mL ethyl acetate and washed with 100 mL 10% citric acid(aq) twice, 100 mL 5% NaHCO3(aq) twice and 100 mL brine twice, dried over MgSO4, and evaporated in vacuum to get about 9 g light yellow oily Ac-Gly-Sar-OBzl c. The mixture was filtered removed THF in vacuum The concentrated residue was dissolved in 100 mL ethyl acetate washed with 100 mL 10% citric acid(aq) twice 100 mL 5% NaHCO3(aq) twice and 100 mL brine twice, dried over MgSO4 evaporated in vacuum
ソース ID: ord-9456afc046e5498fa2a63a0f51eb0d90反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-0ea382043e6642be93dc1fb60719a963反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: A mixture of sarcosine benzyl ester (3.0 g, 30.7 mmol) and succinic anhydride (5.5 g, 30.7 mmol) in toluene (75 mL) was heated to reflux for 3 h, cooled, filtered, and the filtrate was concentrated. The residue was taken up in 5% aqueous sodium carbonate and extracted with ethyl acetate. The aqueous phase was adjusted to pH 3 with concentrated hydrochloric using Congo Red paper and extracted with ethyl acetate. The organic phase was washed with water, dried (magnesium sulfate) and concentrated to yield the title compound (7.4 g, 67.5%): TLC Rf 0.48 (silica, 9:1:1 dichloromethane:methanol:formic acid). was heated to reflux for 3 h cooled filtered the filtrate was concentrated extracted with ethyl acetate with concentrated hydrochloric extracted with ethyl acetate The organic phase was washed with water dried (magnesium sulfate) concentrated
ソース ID: ord-ccae603003f14fca9668b5a8da6d0d4dPubChem References
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