Cyclopentanol → Cyclopentyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

HRID 1700365ノート

反応式

HRID 1700365 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[C:5]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]1[CH:10]([C:16]3([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:19][CH2:18][CH2:17]3)[NH:9][CH2:8][CH2:7][C:6]2=1.[CH:25]1(O)[CH2:29]CC[CH2:26]1>O.CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-].[Ti+4]>[ClH:2].[Cl:2][C:3]1[CH:4]=[C:5]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11]1[CH:10]([C:16]3([C:20]([O:22][CH:23]4[CH2:29][CH2:25][CH2:26][CH2:24]4)=[O:21])[CH2:17][CH2:18][CH2:19]3)[NH:9][CH2:8][CH2:7][C:6]2=1

参加物

5

反応物 2

HCID 7298CyclopentanolHCID 18317933Ethyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

生成物 1

HCID 18317862Cyclopentyl 1-(6-chloro-2,3,4,9-tetrahydro-1H-beta-carbolin-1-yl)cyclobutanecarboxylate Hydrochloride

試薬・触媒・溶媒 2

HCID 11026Titanium isopropoxide触媒HCID 962Water溶媒

実験手順

4.0 g of the compound of Example 1 are heated at the reflux of 80 ml of cyclopentanol in the presence of 1 ml of titanium tetraisopropoxide. After reaction for 24 hours, the reaction mixture is diluted with water and then filtered. After extraction with dichloromethane, drying and evaporation under reduced pressure, crystallisation of the residue from an ethanol-diethyl ether-hydrogen chloride mixture enables the expected product to be isolated.

後処理

  1. customAfter reaction for 24 hours
  2. filtrationfiltered
  3. extractionAfter extraction with dichloromethane
  4. customdrying
  5. customevaporation
  6. customunder reduced pressure, crystallisation of the residue from an ethanol-diethyl ether-hydrogen chloride mixture
  7. customto be isolated

出典と根拠

ORDレコード
ord-e4421ef6078f48b99198835e66621569
出典データセット
uspto-grants-2002_02
特許番号
US06350757B1

反応ノート

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