Ammonia → 1-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea

HRID 1803145ノート

反応式

HRID 1803145 の反応式
[NH3:1].[N:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[N:13][N:14]([CH3:16])[CH:15]=2)=[C:7]([O:17][CH3:18])[CH:6]=1)=[C:3]=[S:4]>>[CH3:18][O:17][C:7]1[CH:6]=[C:5]([NH:2][C:3]([NH2:1])=[S:4])[CH:10]=[CH:9][C:8]=1[C:11]1[CH:12]=[N:13][N:14]([CH3:16])[CH:15]=1

参加物

3

反応物 2

HCID 222AmmoniaHCID 866499074-(4-isothiocyanato-2-methoxyphenyl)-1-methyl-1H-pyrazole

生成物 1

HCID 866499081-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea収率 86.5%

実験手順

Step K (4): Methanolic ammonia (2.0 M, 20 mL, 40 mmol) was added to a flask charged with 4-(4-isothiocyanato-2-methoxyphenyl)-1-methyl-1H-pyrazole (1.46 g, 5.95 mmol). After 3 h, the reaction mixture was concentrated in vacuo. The solid was triturated with diethyl ether. The solid was collected by vacuum filtration and dried under high vacuum to afford 1-(3-methoxy-4-(1-methyl-1H-pyrazol-4-yl)phenyl)thiourea (1.35 g, 86% yield). LC-MS (M+H)+ 263.1.

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. customThe solid was triturated with diethyl ether
  3. filtrationThe solid was collected by vacuum filtration
  4. customdried under high vacuum

出典と根拠

ORDレコード
ord-1867edefc8ae481fa0338eba781a3c70
出典データセット
uspto-grants-2013_01
特許番号
US08349880B2

反応ノート

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