Dichloromethane → HCID 67917948, 화합물

HRID 1682012노트

반응식

HRID 1682012 반응식
[NH:1]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]([CH2:8][N:9]2[C:15](=[O:16])[CH2:14][C:13]3[CH:17]=[C:18]([O:23][CH3:24])[C:19]([O:21][CH3:22])=[CH:20][C:12]=3[CH2:11][CH2:10]2)[CH2:2]1.[CH3:25][O:26][C:27]1[CH:28]=[C:29]([CH2:35][CH2:36]Br)[CH:30]=[CH:31][C:32]=1[O:33][CH3:34].C(Cl)[Cl:39]>C(N(CC)CC)C.[OH-].[Na+]>[ClH:39].[CH3:25][O:26][C:27]1[CH:28]=[C:29]([CH2:35][CH2:36][N:1]2[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]([CH2:8][N:9]3[C:15](=[O:16])[CH2:14][C:13]4[CH:17]=[C:18]([O:23][CH3:24])[C:19]([O:21][CH3:22])=[CH:20][C:12]=4[CH2:11][CH2:10]3)[CH2:2]2)[CH:30]=[CH:31][C:32]=1[O:33][CH3:34]

참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 114706023,4-Dimethoxyphenethyl bromideHCID 198037373-[(hexahydro-azepin-3-yl)-methyl]-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one

생성물 1

HCID 67917948HCID 67917948, 화합물

시약·촉매·용매 2

HCID 8471Triethylamine용매HCID 14798Sodium Hydroxide용매

실험 절차

660 mg (2 mmol) of 3-[(hexahydro-azepin-3-yl)-methyl]-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one and 540 mg (2.2 mmol) of 2-(3,4-dimethoxyphenyl)-ethylbromide are refluxed for 1 hour in 3 ml of triethylamine. The reaction mixture is cooled and taken up in methylene chloride and 2-molar sodium hydroxide solution. The alkaline phase is separated off and extracted twice with methylene chloride. The combined organic phases are dried over magnesium sulphate and evaporated down in vacuo. Purification is carried out by column chromatography over 100 g of aluminium oxide (activity II, eluant: methylene chloride+0.3% ethanol). The fractions obtained are concentrated by evaporation in vacuo, the residue is dissolved in acetone and the hydrochloride is precipitated using ethereal hydrochloric acid.

후처리

  1. temperatureThe reaction mixture is cooled
  2. customThe alkaline phase is separated off
  3. extractionextracted twice with methylene chloride
  4. dry with materialThe combined organic phases are dried over magnesium sulphate
  5. customevaporated down in vacuo
  6. customPurification
  7. customThe fractions obtained
  8. concentrationare concentrated by evaporation in vacuo
  9. dissolutionthe residue is dissolved in acetone
  10. customthe hydrochloride is precipitated

출처 및 근거

ORD 기록
ord-8b254e0fa187429bbc5b9ce8b6d1c3ab
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175157

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