Water → HCID 20433685、化合物

HRID 1154676

反応式

[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

参加物

実験手順

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.

後処理

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

出典と根拠

ORDレコード: ord-ad6624aec3ba45f5bf0598f0c6d817dc
出典データセット: uspto-grants-1984_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04490369

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート