Hydrogen Bromide → HCID 86603179、化合物

HRID 1818950ノート

反応式

HRID 1818950 の反応式
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

参加物

6

反応物 3

HCID 260Hydrogen BromideHCID 15891Phenyl chloroformateHCID 144238482-[2-(2-Amino-1,3-thiazol-5-yl)ethyl]-1H-isoindole-1,3(2H)-dione2 回

生成物 1

HCID 86603179HCID 86603179、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9df3f51748514daa85919b77ffbabba9
出典データセット
uspto-grants-2009_10
特許番号
US07601725B2

反応ノート

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