3-Pyridinemethanamine → 4-[4-Chloro-3-(3-picolylsulfamoyl)-phenyl]-3-methyl-2-methylimino-1,3-thiazolidine-4-ol

HRID 461190노트

반응식

HRID 461190 반응식
Br.[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([OH:17])[CH2:13][S:12][C:11](=[N:14][CH3:15])[N:10]2[CH3:16])=[CH:5][C:4]=1[S:18](Cl)(=[O:20])=[O:19].[N:22]1[CH:27]=[CH:26][CH:25]=[C:24]([CH2:28][NH2:29])[CH:23]=1>C(N(CC)CC)C>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([OH:17])[CH2:13][S:12][C:11](=[N:14][CH3:15])[N:10]2[CH3:16])=[CH:5][C:4]=1[S:18](=[O:20])(=[O:19])[NH:29][CH2:28][C:24]1[CH:23]=[N:22][CH:27]=[CH:26][CH:25]=1

참가 물질

4

반응물 2

HCID 310183-PyridinemethanamineHCID 227604894-Chloro-3-chlorosulfonylphenyl-3-methyl-2-methylimino-1,3-thiazolidine-4-ol-hydrobromide

생성물 1

HCID 227606964-[4-Chloro-3-(3-picolylsulfamoyl)-phenyl]-3-methyl-2-methylimino-1,3-thiazolidine-4-ol

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

8.8 g of 4-(4-chloro-3-chlorosulfonylphenyl)-3-methyl-2-methylimino-1,3-thiazolidine-4-ol-hydrobromide were reacted with 3.0 g of 3-picolyl amine and 5 g of triethyl amine according to Example 76, the solvent was distilled off under reduced pressure and the residue was taken up in 70 ml of water. Three extractions followed with 60 ml of ethyl acetate, the organic phase was dried over sodium sulfate and the solvent was evaporated under reduced pressure. The residue crystallized under diisopropyl ether. Melting point: 152° - 153° C.

후처리

  1. distillationthe solvent was distilled off under reduced pressure
  2. extractionThree extractions
  3. dry with materialthe organic phase was dried over sodium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue crystallized under diisopropyl ether

출처 및 근거

ORD 기록
ord-86948021a7bb48a599e8f28e04833188
출처 데이터셋
uspto-grants-1977_12
특허 번호
US04061761

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