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

HRID 1703919노트

반응식

HRID 1703919 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-5ac1b072048b43a39da444e26ac827c1
출처 데이터셋
uspto-grants-1978_11
특허 번호
US04125614

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