Hexane → N-(6-Chloro-3-methoxy-2-pyridinyl)-N'-carboethoxythiourea

HRID 1940927노트

반응식

HRID 1940927 반응식
[CH2:1]([O:3][C:4]([N:6]=[C:7]=[S:8])=[O:5])[CH3:2].[NH2:9][C:10]1[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([Cl:18])[N:11]=1.CCCCCC>C(Cl)(Cl)Cl>[Cl:18][C:12]1[N:11]=[C:10]([NH:9][C:7]([NH:6][C:4]([O:3][CH2:1][CH3:2])=[O:5])=[S:8])[C:15]([O:16][CH3:17])=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 8058HexaneHCID 85320Ethyl isothiocyanatoformateHCID 214643776-Chloro-3-methoxypyridin-2-amine

생성물 1

HCID 21464341N-(6-Chloro-3-methoxy-2-pyridinyl)-N'-carboethoxythiourea수율 90.9%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

Ethoxycarbonyl isothiocyanate (3.7 mL, 4.1 g, 31.5 mmol) was added slowly with stirring to a solution of 2-amino-6-chloro-3-methoxypyridine (5.0 g, 31.5 mmol) in chloroform (40 mL) and the mixture was stirred overnight. The solvent was removed by evaporation and the residue obtained was mixed with hexane. The resulting slurry was filtered and the solids collected were washed with a small amount of ether and dried to obtain 8.3 g of the title compound as a man powder melting at 184°-185° C. with decomposition.

후처리

  1. customThe solvent was removed by evaporation
  2. customthe residue obtained
  3. filtrationThe resulting slurry was filtered
  4. customthe solids collected
  5. washwere washed with a small amount of ether
  6. customdried

출처 및 근거

ORD 기록
ord-b5086040948c4118893ce8615ca37adf
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700940

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