Water → 4-bromo-1-(4-nitrobenzoyl)-3,4-dihydro-1H-benzo[b]azepin-5(2H)-one

HRID 355875

反応式

HRID 355875 の反応式
[N+:1]([C:4]1[CH:23]=[CH:22][C:7]([C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[C:14](=[O:21])[CH2:13][CH2:12][CH2:11]2)=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].[Br:24]Br.O>C(O)(=O)C>[Br:24][CH:13]1[C:14](=[O:21])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[N:10]([C:8](=[O:9])[C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:23][CH:22]=2)[CH2:11][CH2:12]1

参加物

5

反応物 3

HCID 962WaterHCID 24408BromineHCID 107337295H-1-Benzazepin-5-one, 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-

生成物 1

HCID 540926514-bromo-1-(4-nitrobenzoyl)-3,4-dihydro-1H-benzo[b]azepin-5(2H)-one収率 87.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

A mixture of 0.200 g of 1,2,3,4-tetrahydro-1-(4-nitrobenzoyl)-5H-1-benzazepin-5-one in 2.5 ml of acetic acid is warmed until solution then allowed to cool to room temperature. While stirring, a solution of 0.103 g of bromine in 0.5 ml of acetic acid is added dropwise. After rapid decolorization, the reaction mixture is stirred for 1.5 hours and poured into water. The solid is collected, washed with water and air dried to give 220 mg of the desired product as a crystalline solid, Mass Spectrum; MH+ =389,391.

後処理

  1. temperatureis warmed until solution
  2. stirringAfter rapid decolorization, the reaction mixture is stirred for 1.5 hours
  3. customThe solid is collected
  4. washwashed with water and air
  5. customdried

出典と根拠

ORDレコード
ord-11a00db90ee6472cae5b37ac1a7b4021
出典データセット
uspto-grants-1998_11
特許番号
US05834461

関連ノート

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