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Methyl Isocyanate → N-methyl-N'-(4-(1-(2-fluoro-4-biphenylyl)ethyl)thiazol-2-yl)urea

HRID 974052
ノート
印刷プレビュー

反応式

HRID 974052 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH:7]([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:11]([F:21])[CH:10]=2)[CH3:8])[N:6]=1.[CH3:22][N:23]=[C:24]=[O:25]>C(Cl)(Cl)Cl>[CH3:22][NH:23][C:24]([NH:1][C:2]1[S:3][CH:4]=[C:5]([CH:7]([C:9]2[CH:14]=[CH:13][C:12]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)=[C:11]([F:21])[CH:10]=2)[CH3:8])[N:6]=1)=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12228Methyl Isocyanate2 回HCID 104699822-Amino-4-(1-(2-fluoro-4-biphenylyl)ethyl)thiazole

生成物 1

HCID 15676061N-methyl-N'-(4-(1-(2-fluoro-4-biphenylyl)ethyl)thiazol-2-yl)urea収率 84%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

To 2-amino-4-(1-(2-fluoro-4-biphenylyl)ethyl) thiazole (500 mg, 1.68 mmol) in chloroform (20 ml) was added methylisocyanate (0.10 mg, 1.75 mmol) in chloroform (10 ml) under cooling with ice. After the mixture was stirred, methylisocyanate (0.15 mmol, 2.63 mmol) was added to the mixture, and then the mixture was stirred at room temperature overnight. The mixture was evaporated under reduced pressure to a residue, which was crystallized to afford N-methyl-N'-(4-(1-(2-fluoro-4-biphenylyl)ethyl) thiazol-2-yl)urea (0.499 g, 84% yield) as crystalline material: mp 208.5°-209.0° C.

後処理

  1. temperatureunder cooling with ice
  2. stirringthe mixture was stirred at room temperature overnight
  3. customThe mixture was evaporated under reduced pressure to a residue, which
  4. customwas crystallized

出典と根拠

ORDレコード
ord-abe49ba4bdf2418ab4f36bd76dfbf9b6
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05066666

反応ノート

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