Hydrogen Bromide → HCID 86603179, 화합물

HRID 1818950노트

반응식

HRID 1818950 반응식
Br.[NH2:2][C:3]1[S:4][C:5]([CH2:8][CH2:9][N:10]2[C:18](=[O:19])[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]2=[O:20])=[CH:6][N:7]=1.Cl[C:22]([O:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=[O:23]>ClCCl.CCOC(C)=O>[C:25]1([O:24][C:22](=[O:23])[NH:2][C:3]2[S:4][C:5]([CH2:8][CH2:9][N:10]3[C:18](=[O:19])[C:17]4[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=4)[C:11]3=[O:20])=[CH:6][N:7]=2)[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

참가 물질

6

반응물 3

HCID 260Hydrogen BromideHCID 15891Phenyl chloroformateHCID 144238482-[2-(2-Amino-1,3-thiazol-5-yl)ethyl]-1H-isoindole-1,3(2H)-dione2회

생성물 1

HCID 86603179HCID 86603179, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

To a suspension of a HBr salt of 2-[2-(2-amino-thiazol-5-yl)-ethyl]-isoindole-1,3-dione (compound 58.1; 1.42 mmol) in dichloromethane was added TEA (4.30 mmol) followed by the addition of phenyl chloroformate (1.43 mmol) at room temperature. After 2 hours, the reaction was concentrated to dryness to give a solid that was suspended in EtOAc, filtered, washed with additional EtOAc and dried under vacuum to provide {5-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-ethyl]-thiazol-2-yl}-carbamic acid phenyl ester (compound 58.2, which is contaminated with triethyl amine salts) which was used in the next reaction without further purification.

후처리

  1. concentrationthe reaction was concentrated to dryness
  2. customto give a solid
  3. filtrationfiltered
  4. washwashed with additional EtOAc
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-9df3f51748514daa85919b77ffbabba9
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601725B2

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