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

HRID 1940927ノート

反応式

HRID 1940927 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b5086040948c4118893ce8615ca37adf
出典データセット
uspto-grants-1997_12
特許番号
US05700940

反応ノート

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