2-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl ester → HCID 20261265、化合物

HRID 464913

反応式

HRID 464913 の反応式
[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[S:10]([N:13]=[C:14]=[O:15])(=[O:12])=[O:11])=[O:4].[NH2:16][C:17]1[N:22]=[C:21]([O:23][CH:24]([F:26])[F:25])[CH:20]=[C:19]([CH3:27])[N:18]=1>O1CCCC1>[CH3:1][O:2][C:3]([C:5]1[S:6][CH:7]=[CH:8][C:9]=1[S:10]([NH:13][C:14]([NH:16][C:17]1[N:22]=[C:21]([O:23][CH:24]([F:26])[F:25])[CH:20]=[C:19]([CH3:27])[N:18]=1)=[O:15])(=[O:12])=[O:11])=[O:4]

参加物

4

反応物 2

HCID 1572962-Thiophenecarboxylic acid, 3-(isocyanatosulfonyl)-, methyl esterHCID 28173904-(Difluoromethoxy)-6-methylpyrimidin-2-amine

生成物 1

HCID 20261265HCID 20261265、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 6.2 g of 2-methoxycarbonyl-3-thienylsulfonylisocyanate in 50 ml of absolute tetrahydrofuran is stirred dropwise into a solution of 4.4 g of 2-amino-4-difluoromethoxy-6-methylpyrimidine in 80 ml of absolute tetrahydrofuran. During the course of this addition, the temperature of the reaction mixture rises from 20° to 26° C. After it has been stirred for another hour, the raction mixture is filtered and the filtrate is concentrated. The residue is crystallised from ethyl acetate, affording 5.3 g (50%) of N-(2-methoxycarbonyl-3-thienylsulfonyl)-N'-(4-difluoromethoxy-6-methylpyrimidin-2-yl)urea (compound 2.1) with a melting point of 178°-179° C.

後処理

  1. additionDuring the course of this addition
  2. customrises from 20° to 26° C
  3. filtrationthe raction mixture is filtered
  4. concentrationthe filtrate is concentrated
  5. customThe residue is crystallised from ethyl acetate

出典と根拠

ORDレコード
ord-3086ea1c378a4a7e855846d0a83f48ec
出典データセット
uspto-grants-1985_10
特許番号
US04549898

関連ノート

読み込み中…