HCID 86689231、化合物 → HCID 71621925、化合物

HRID 871022ノート

反応式

HRID 871022 の反応式
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-])=[O:14])[CH:8]=2)[C:3]=1[C:16]([NH2:18])=[O:17].[H][H]>CO.[Pt]=O>[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([NH:13][OH:14])[CH:8]=2)[C:3]=1[C:16]([NH2:18])=[O:17]

参加物

5

反応物 2

HCID 86689231HCID 86689231、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 71621925HCID 71621925、化合物収率 67.3%

試薬・触媒・溶媒 2

HCID 82844Platinum oxide (PtO)触媒2 回HCID 887Methanol溶媒

実験手順

A mixture of 5-amino-3-(3-nitrophenyl)isothiazole-4-carboxamide (50 mg, 0.19 mmol) and platinum oxide (20 mg, 0.088 mmol) in 5 mL MeOH was hydrogenated under 60 PSI hydrogen. After 5 hours an additional catalytic amount of platinum oxide was added and the reaction continued for 67 hours. The reaction mixture was filtered using Celite and the filter bed rinsed with 40% MeOH/CHCl3. The filtrate was evaporated to give 32 mg of yellow solid. Then 22 mg of this material was chromatographed eluting with CHCl3/MeOH to give the title compound as a pale yellow solid (10.2 mg).

後処理

  1. filtrationThe reaction mixture was filtered
  2. washthe filter bed rinsed with 40% MeOH/CHCl3
  3. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-b6951dc5e0bc420f9bf66f7455cb855c
出典データセット
uspto-grants-2015_03
特許番号
US08969583B2

反応ノート

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