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Triethylamine → HCID 13319934, 화합물

HRID 1154682
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HRID 1154682 반응식
[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][Cl:15])[CH2:10][CH2:11][C:5]=2[CH:4]=1.C(N(CC)CC)C.[CH3:28][NH:29][CH2:30][CH2:31][CH2:32][C:33]1[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=1>C(Cl)Cl.O.CC(C)=O>[ClH:15].[CH3:1][O:2][C:3]1[C:18]([O:19][CH3:20])=[CH:17][C:6]2[CH2:7][C:8](=[O:16])[N:9]([CH2:12][CH2:13][CH2:14][N:29]([CH3:28])[CH2:30][CH2:31][CH2:32][C:33]3[CH:38]=[CH:37][C:36]([O:39][CH3:40])=[C:35]([O:41][CH3:42])[CH:34]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 7131256N-[3-(3,4-dimethoxyphenyl)propyl]-N-methylamineHCID 130925103-(3-Chloropropyl)-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one

생성물 1

HCID 13319934HCID 13319934, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 21908982
Water methylene chloride
용매

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온도
85 °C

실험 절차

A mixture of 5.55 gm (0.0186 mol) of 1-[7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl]-3-chloro-propane, 2.6 ml (0.0886 mol) of triethylamine and 3.9 gm (0.0186 mol) of N-methyl-3-(3,4-dimethoxy-phenyl) propylamine was heated at 85° C. for 4 hours, then cooled and dissolved in methylene chloride/water. The organic phase was separated, extracted with water, dried over magnesium sulfate, concentrated by evaporation in vacuo, and the residue was purified on silica gel, using methylene chloride plus 3% ethanol as the eluant. The oily free base product thus obtained was dissolved in acetone, and the hydrochloride was precipitated with ethereal hydrochloric acid.

후처리

  1. temperaturecooled
  2. customThe organic phase was separated
  3. extractionextracted with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated by evaporation in vacuo
  6. customthe residue was purified on silica gel
  7. customThe oily free base product thus obtained
  8. customthe hydrochloride was precipitated with ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-74f942d0bc2243a392b182cd56219b63
출처 데이터셋
uspto-grants-1984_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04490369

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