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

HRID 971612노트

반응식

HRID 971612 반응식
[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]

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 12668015HCID 12668015, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 712Formaldehyde용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-536100f5df4f4cb1a94ee60a712b0aeb
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04160765

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