Water → HCID 20433685, 화합물

HRID 1154676

반응식

HRID 1154676 반응식
[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[NH:9][CH2:10][CH2:11][C:5]=2[CH:4]=1.[Cl:17][CH2:18][CH2:19][CH2:20][N:21]([CH3:34])[CH2:22][CH2:23][C:24]1[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=1.O>CS(C)=O>[ClH:17].[ClH:17].[CH3:1][O:2][C:3]1[C:14]([O:15][CH3:16])=[CH:13][C:6]2[CH2:7][C:8](=[O:12])[N:9]([CH2:18][CH2:19][CH2:20][N:21]([CH3:34])[CH2:22][CH2:23][C:24]3[CH:29]=[CH:28][C:27]([O:30][CH3:31])=[C:26]([O:32][CH3:33])[CH:25]=3)[CH2:10][CH2:11][C:5]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 577693N-(3-Chloropropyl)-3,4-dimethoxy-N-methylphenethylamineHCID 114017697,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepin-2-one

생성물 1

HCID 20433685HCID 20433685, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

1.1 gm (5.0 mmols) of 7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one were suspended in 20 ml of dimethyl sulfoxide, and the suspension was mixed with 0.6 gm (5.3 mmols) of potassium tert. butylate while stirring. After 10 minutes, the solution was mixed with 2.0 gm (7.4 mmols) of 1-chloro-3-[N-methyl-N-(2-{3,4-dimethoxy-phenyl}-ethyl)-amino]-propane; the mixture was stirred for one hour at 50° C. and then poured into water; the aqueous mixture was extracted with ethyl acetate, and the organic phase was evaporated in vacuo. The residue was purified on silica gel with methylene chloride +10% of methanol as the eluant, and the dihydrochloride was precipitated from acetone with ethereal hydrochloric acid.

후처리

  1. stirringthe mixture was stirred for one hour at 50° C.
  2. extractionthe aqueous mixture was extracted with ethyl acetate
  3. customthe organic phase was evaporated in vacuo
  4. customThe residue was purified on silica gel with methylene chloride +10% of methanol as the eluant
  5. customthe dihydrochloride was precipitated from acetone with ethereal hydrochloric acid

출처 및 근거

ORD 기록
ord-ad6624aec3ba45f5bf0598f0c6d817dc
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04490369

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