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HCID 9858173、化合物 → HCID 9879038、化合物

HRID 1744025
ノート
印刷プレビュー

反応式

HRID 1744025 の反応式
[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH2:14][CH2:15][CH2:16][C:17]([CH3:22])([N+:19]([O-])=O)[CH3:18])[C:10]([O:12][CH3:13])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO.[Fe]>[CH3:13][O:12][C:10](=[O:11])[C@H:9]([CH2:14][CH2:15][CH2:16][C:17]([CH3:22])([CH3:18])[NH2:19])[NH:8][C:6]([O:5][C:1]([CH3:4])([CH3:2])[CH3:3])=[O:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 9858173HCID 9858173、化合物

生成物 1

HCID 9879038HCID 9879038、化合物収率 55%

試薬・触媒・溶媒 2

HCID 23925Iron触媒2 回HCID 887Methanol溶媒

反応条件

温度
40 °C

実験手順

Methyl (S)-2-t-butoxycarbonylamino-6-methyl-6-nitroheptanoate (10.05 g, 31.6 mmol) was dissolved in methanol (200 ml). Iron powder (8.81 g, 157.8 mmol) and ferrous sulfate 7 hydrate (40.5 g, 145.6 mmol) were added and the mixture was stirred at 40° C. for 17 h. Since the starting material remained, the insoluble matter was removed by filtration. Iron powder (8.81 g, 157.8 mmol) and ferrous sulfate 7 hydrate (40.5 g, 145.6 mmol) were added and the mixture was stirred at 40° C. for 7 h. The insoluble material was removed by filtration, and methanol was removed by concentration under reduced pressure. Ethyl acetate (300 ml), water (100 ml) and 10% aqueous sodium carbonate solution were added for pH adjustment to 9 and extraction. Ethyl acetate was evaporated by concentration under reduced pressure to give the objective compound (5.01 g, yield 55.0%).

後処理

  1. customthe insoluble matter was removed by filtration
  2. stirringthe mixture was stirred at 40° C. for 7 h
  3. customThe insoluble material was removed by filtration, and methanol
  4. customwas removed by concentration under reduced pressure
  5. additionEthyl acetate (300 ml), water (100 ml) and 10% aqueous sodium carbonate solution were added for pH adjustment to 9 and extraction
  6. customEthyl acetate was evaporated by concentration under reduced pressure

出典と根拠

ORDレコード
ord-76abcb8686d647ba908646f591e666ed
出典データセット
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07012152B2

反応ノート

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