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

HRID 1866550ノート

反応式

HRID 1866550 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3506092baba04f239831d82bb5456718
出典データセット
uspto-grants-2009_12
特許番号
US07629358B2

反応ノート

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