Nitric Acid → HCID 22030612、化合物

HRID 454309

反応式

HRID 454309 の反応式
C[O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6]2.[N+:17]([O-])([OH:19])=[O:18]>ClCCl>[OH:2][C:3]1[C:4]([N+:17]([O-:19])=[O:18])=[C:5]2[C:9](=[CH:10][CH:11]=1)[NH:8][C:7]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6]2

参加物

4

反応物 2

HCID 944Nitric AcidHCID 20926Ethyl 5-methoxyindole-2-carboxylate

生成物 1

HCID 22030612HCID 22030612、化合物収率 59%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of ethyl 5-methoxyindole-2-carboxylate (8.15 g, 37.2 mmol), (prepared by the method described in Heterocycles Vol. 43, No. 2, p. 263-266), nitric acid adsorbed on silica gel (24 g) and dichloromethane (150 ml) was stirred at ambient temperature for 18 hours. The dichloromethane was removed in vacuo and the product washed off the silica with acetone. The acetone was evaporated in vacuo. The residue was treated again with nitric acid on silica (1 g) as above and the work up procedure repeated to give ethyl 5-hydroxy-4-nitroindole-2-carboxylate (5.8 g, 59%).

後処理

  1. custom(prepared by the method
  2. customThe dichloromethane was removed in vacuo
  3. washthe product washed off the silica with acetone
  4. customThe acetone was evaporated in vacuo
  5. additionThe residue was treated again with nitric acid on silica (1 g) as above and the work up procedure

出典と根拠

ORDレコード
ord-132ad3e4bce44edb80e78c38a37e2a70
出典データセット
uspto-grants-2013_07
特許番号
US08492560B2

関連ノート

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