Ethanol → HCID 21478799、化合物

HRID 1604629ノート

反応式

HRID 1604629 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([N+:22]([O-])=O)=[C:13]([CH2:15][C:16]([O:18][CH:19]([CH3:21])[CH3:20])=[O:17])[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+].C(O)C>[Fe].O>[NH2:22][C:12]1[CH:11]=[CH:10][C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[CH:14][C:13]=1[CH2:15][C:16]([O:18][CH:19]([CH3:21])[CH3:20])=[O:17]

参加物

6

反応物 3

HCID 702EthanolHCID 25517Ammonium ChlorideHCID 19603840HCID 19603840、化合物

生成物 1

HCID 21478799HCID 21478799、化合物収率 102.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of isopropyl 5-benzyloxy-2-nitrophenylacetate (4.2 g), ammonium chloride (0.42 g) and iron powder (4.2 g) in a mixed solvent of ethanol (20 ml) and water (10 ml) was stirred at 80° C. for 1.2 hours. After cooling, the reaction mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was partitioned between water and ethyl acetate and the ethyl acetate layer was washed with brine, dried over magnesium sulfate and evaporated under reduced pressure to give isopropyl 2-amino-5-benzyloxyphenylacetate (3.9 g).

後処理

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was partitioned between water and ethyl acetate
  5. washthe ethyl acetate layer was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-482e9a04746b4307a72df8d58c9fc0b7
出典データセット
uspto-grants-1999_11
特許番号
US05994378

反応ノート

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