Acetic Acid → 3-Amino-4-methoxyphenyl ethyl carbonate

HRID 1776587ノート

反応式

HRID 1776587 の反応式
[C:1](=[O:17])([O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([N+:14]([O-])=O)[CH:7]=1)[O:2][CH2:3][CH3:4].C(O)(=O)C>CCOC(C)=O.[Pd]>[C:1](=[O:17])([O:2][CH2:3][CH3:4])[O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([NH2:14])[CH:7]=1

参加物

5

反応物 2

HCID 176Acetic AcidHCID 86679539Ethyl 4-methoxy-3-nitrophenyl carbonate

生成物 1

HCID 134556543-Amino-4-methoxyphenyl ethyl carbonate収率 95%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl 4-methoxy-3-nitrophenyl carbonate (0.720 g, 2.99 mmol) was dissolved in EtOAc (20 ml), and glacial acetic acid (0.200 ml, 3.49 mmol) was added followed by 10% palladium on carbon (0.100 g, 0.094 mmol). The mixture was stirred in a Parr apparatus under hydrogen atmosphere (25 psi) for 2 hours. The catalyst was filtered off, and the filtrate was evaporated under reduced pressure. The resulting crude 3-amino-4-methoxyphenyl ethyl carbonate (0.600 g, 2.84 mmol, 95% yield, MS/ESI+ 212.3 [MH]+), was used for the next step without any further purification.

後処理

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-62a3e974e4604c02bc81588776331c5b
出典データセット
uspto-grants-2016_02
特許番号
US09265768B2

反応ノート

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