Trifluoroacetic acid → 3-[3-(2-Amino-2-methyl-propyl)phenyl]-acrylic acid benzyl ester

HRID 1866550노트

반응식

HRID 1866550 반응식
[CH2:1]([O:8][C:9](=[O:30])[CH:10]=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][C:19]([NH:22]C(OC(C)(C)C)=O)([CH3:21])[CH3:20])[CH:13]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>ClCCl>[CH2:1]([O:8][C:9](=[O:30])[CH:10]=[CH:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][C:19]([NH2:22])([CH3:20])[CH3:21])[CH:13]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 690235023-[3-(2-tert-Butoxycarbonylamino-2-methyl-propyl)-phenyl]-acrylic acid benzyl ester

생성물 1

HCID 690261303-[3-(2-Amino-2-methyl-propyl)phenyl]-acrylic acid benzyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 3-[3-(2-tert-butoxycarbonylamino-2-methyl-propyl)-phenyl]-acrylic acid benzyl ester (preparation 141), (2.23 g, 5.45 mmol), and trifluoroacetic acid (5 mL) in dichloromethane (10 mL) was stirred for 1 hour at room temperature. The mixture was then concentrated in vacuo and the residue was diluted with sodium hydrogen carbonate solution (10 mL) and extracted with ethyl acetate (3×20 mL). The combined organic solution was dried over magnesium sulfate and concentrated in vacuo to afford the title compound as a yellow oil in quantitative yield.

후처리

  1. concentrationThe mixture was then concentrated in vacuo
  2. additionthe residue was diluted with sodium hydrogen carbonate solution (10 mL)
  3. extractionextracted with ethyl acetate (3×20 mL)
  4. dry with materialThe combined organic solution was dried over magnesium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-3506092baba04f239831d82bb5456718
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629358B2

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