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

HRID 1700365노트

반응식

HRID 1700365 반응식
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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 11026Titanium isopropoxide촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e4421ef6078f48b99198835e66621569
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06350757B1

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