Formic Acid → 6-Chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

HRID 971612ノート

反応式

HRID 971612 の反応式
[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][NH:9][CH2:8][CH:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:5]=[C:4]([O:19][CH3:20])[C:3]=1[O:21][CH3:22].[OH-].[Na+].[CH:25](O)=O>C=O>[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][N:9]([CH3:25])[CH2:8][CH:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:6]=2[CH:5]=[C:4]([O:19][CH3:20])[C:3]=1[O:21][CH3:22]

参加物

5

反応物 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 12668015HCID 12668015、化合物

生成物 1

HCID 4359706-Chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine

試薬・触媒・溶媒 1

HCID 712Formaldehyde溶媒

実験手順

A solution of 3.7 g of 6-chloro-7,8-dimethoxy-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine in 15 ml of formic acid and 10 ml of formaldehyde is refluxed for 18 hours. The reaction mixture is evaporated to dryness, 20 ml of 6N hydrochloric acid is added and the solution is again evaporated to dryness to give a liquid. The latter is treated with 20 ml of 10% sodium hydroxide solution and the mixture is extracted with ether. The dried extract is evaporated to give 6-chloro-7,8-dimethoxy-3-methyl-1-phenyl-2,3,4,5-tetrahydro-1H-3-benzazepine.

後処理

  1. customThe reaction mixture is evaporated to dryness, 20 ml of 6N hydrochloric acid
  2. additionis added
  3. customthe solution is again evaporated to dryness
  4. customto give a liquid
  5. extractionthe mixture is extracted with ether
  6. extractionThe dried extract
  7. customis evaporated

出典と根拠

ORDレコード
ord-536100f5df4f4cb1a94ee60a712b0aeb
出典データセット
uspto-grants-1979_07
特許番号
US04160765

反応ノート

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