2-Amino-5-methylthiazole → 2,6-Dimethyl-4-hydroxy-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide

HRID 224599노트

반응식

HRID 224599 반응식
[OH:1][C:2]1[C:7]2[CH:8]=[C:9]([CH3:12])[CH:10]=[CH:11][C:6]=2[S:5](=[O:14])(=[O:13])[N:4]([CH3:15])[C:3]=1[C:16]([O:18]C)=O.[NH2:20][C:21]1[S:22][C:23]([CH3:26])=[CH:24][N:25]=1>C1(C)C(C)=CC=CC=1>[CH3:15][N:4]1[C:3]([C:16]([NH:20][C:21]2[S:22][C:23]([CH3:26])=[CH:24][N:25]=2)=[O:18])=[C:2]([OH:1])[C:7]2[CH:8]=[C:9]([CH3:12])[CH:10]=[CH:11][C:6]=2[S:5]1(=[O:13])=[O:14]

참가 물질

4

반응물 2

HCID 3517702-Amino-5-methylthiazoleHCID 54696079methyl 4-hydroxy-2,6-dimethyl-2H-1,2-benzothiazine-3-carboxylate-1,1-dioxide

생성물 1

HCID 546942212,6-Dimethyl-4-hydroxy-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

4.0 gm (14 millimols) of methyl 4-hydroxy-2,6-dimethyl-2H-1,2-benzothiazine-3-carboxylate-1,1-dioxide and 2.0 gm (17 millimols) of 2-amino-5-methyl-thiazole were refluxed in 200 ml of anhydrous xylene for 24 hours. After cooling, the crystals which had separated out were filtered off. After recrystallization from ethylene chloride 3.6 gm (70% of theory) of 2,6-dimethyl-4-hydroxy-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3carboxamide-1,1-dioxide were obtained.

후처리

  1. temperatureAfter cooling
  2. customthe crystals which had separated out
  3. filtrationwere filtered off
  4. customAfter recrystallization from ethylene chloride 3.6 gm (70% of theory) of 2,6-dimethyl-4-hydroxy-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3carboxamide-1,1-dioxide
  5. customwere obtained

출처 및 근거

ORD 기록
ord-193861cfc36a487aa1ee9cd683e467d0
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04233299

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