N-(3-Aminopropyl)morpholine → 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene} methanesulfonylmethyl)-N-(3-morpholin-4-ylpropyl)benzamide

HRID 1058813

반응식

HRID 1058813 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[CH2:10][CH2:9][O:8][CH2:7][CH2:6]1.[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([CH:18]([C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=2)[N:19]2[CH2:22][C:21](=[CH:23][S:24]([CH2:27][C:28]3[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=3)[C:31](O)=[O:32])(=[O:26])=[O:25])[CH2:20]2)=[CH:14][CH:13]=1>ClCCl>[Cl:11][C:12]1[CH:17]=[CH:16][C:15]([CH:18]([C:37]2[CH:38]=[CH:39][C:40]([Cl:43])=[CH:41][CH:42]=2)[N:19]2[CH2:22][C:21](=[CH:23][S:24]([CH2:27][C:28]3[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=3)[C:31]([NH:1][CH2:2][CH2:3][CH2:4][N:5]3[CH2:10][CH2:9][O:8][CH2:7][CH2:6]3)=[O:32])(=[O:26])=[O:25])[CH2:20]2)=[CH:14][CH:13]=1

참가 물질

4

반응물 2

HCID 61055N-(3-Aminopropyl)morpholineHCID 696356783-({1-[Bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)benzoic acid

생성물 1

HCID 696356533-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene} methanesulfonylmethyl)-N-(3-morpholin-4-ylpropyl)benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.0388 cm3 of N-(3-aminopropyl)morpholine is added, at the same temperature, to a suspension of 150 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)benzoic acid activated on TFP resin (165 μM) in 3 cm3 of dichloromethane, pre-stirred for 90 minutes at a temperature close to 20° C. The suspension is stirred at a temperature close to 20° C. for 22 hours and then filtered on sintered glass. The solid residue is rewashed with twice 1.5 cm3 of dichloromethane. The filtrates are combined and concentrated to dryness under reduced pressure (2.7 kPa) at a temperature close to 40° C. 60 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-ylidene}methanesulfonylmethyl)-N-(3-morpholin-4-ylpropyl)benzamide are thus obtained in the form of a pale yellow foam.

후처리

  1. customclose to 20° C
  2. stirringThe suspension is stirred at a temperature
  3. customclose to 20° C. for 22 hours
  4. filtrationfiltered on sintered glass
  5. concentrationconcentrated to dryness under reduced pressure (2.7 kPa) at a temperature
  6. customclose to 40° C

출처 및 근거

ORD 기록
ord-f09eb52bc54a444f83e4dfb3d8ab8a84
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06518264B2

연결된 노트

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