Water → HCID 178484781, 화합물

HRID 1463758

반응식

HRID 1463758 반응식
[Cl:1][C:2]1[C:3]([C:20]#[N:21])=[C:4]([C:13]2[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=2)[N:5](CCl)[C:6]=1[C:7]([F:10])([F:9])[F:8].[CH3:22][N:23]([CH3:27])[C:24](=[S:26])[SH:25].[Na].O.[CH3:30]N(C)C=O>CCCCCC>[Cl:1][C:2]1[C:3]([C:20]#[N:21])=[C:4]([C:13]2[CH:14]=[CH:15][C:16]([Cl:19])=[CH:17][CH:18]=2)[N:5]([SH:26]([CH3:30])[C:24](=[S:25])[N:23]([CH3:27])[CH3:22])[C:6]=1[C:7]([F:8])([F:10])[F:9]

참가 물질

7

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 6599Dimethyldithiocarbamic acidHCID 5360545SodiumHCID 110356014-Chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile

생성물 1

HCID 178484781HCID 178484781, 화합물수율 80%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

A mixture of 4-chloro-1-(chloromethyl)-2-(p-chlorophenyl)-5-(trifluoromethyl)pyrrole-3-carbonitrile (0.7 g, 0.002 mol) and dimethyldithiocarbamic acid, sodium salt (0.57 g, 0.004 mol) in dimethyl formamide is heated at 50°-55° for 30 minutes, cooled to room temperature and poured into water. The resultant mixture is extracted with ethyl acetate. The combined extracts are washed with a saturated sodium chloride solution, dried (MGSO4) and concentrated in vacuo to give an orange oil residue. The residue is mixed with hot hexane, cooled and filtered to give an orange solid filtercake. Recrystallization of the solid from isopropanol gives the title product as a tan crystaline solid, 0.7 g (80% yield), mp 129°-131° C.

후처리

  1. temperatureis heated at 50°-55° for 30 minutes
  2. extractionThe resultant mixture is extracted with ethyl acetate
  3. washThe combined extracts are washed with a saturated sodium chloride solution
  4. customdried (MGSO4)
  5. concentrationconcentrated in vacuo
  6. customto give an orange oil residue
  7. temperaturecooled
  8. filtrationfiltered
  9. customto give an orange solid filtercake
  10. customRecrystallization of the solid from isopropanol

출처 및 근거

ORD 기록
ord-3ff6c4600b284f1e906c2f27781c5579
출처 데이터셋
uspto-grants-1994_04
특허 번호
US05302383

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