Hydrazine hydrate (1:1) → 4-(2-Amino-3-mercaptophenylsulfonamido)benzoic acid

HRID 2202411ノート

反応式

HRID 2202411 の反応式
[S:1]1[C:5]2=[CH:6][CH:7]=[CH:8][C:9]([S:10]([NH:13][C:14]3[CH:22]=[CH:21][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=3)(=[O:12])=[O:11])=[C:4]2[N:3]=C1.O.NN>CCO>[NH2:3][C:4]1[C:5]([SH:1])=[CH:6][CH:7]=[CH:8][C:9]=1[S:10]([NH:13][C:14]1[CH:22]=[CH:21][C:17]([C:18]([OH:20])=[O:19])=[CH:16][CH:15]=1)(=[O:11])=[O:12]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 904189724-(Benzo[d]thiazole-4-sulfonamido)benzoic acid

生成物 1

HCID 904190184-(2-Amino-3-mercaptophenylsulfonamido)benzoic acid収率 92.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
130 °C

実験手順

To a solution of 4-(benzo[d]thiazole-4-sulfonamido)benzoic acid (500 mg, 1.5 mmol) in 6 mL of EtOH was added hydrazine hydrate (479 mg, 15 mmol) at r.t. The reaction mixture was then stirred at 130° C. in microwave for 1.5 h. The resulting mixture was then cooled, and partitioned between water and EtOAc. The organic phase was washed with brine, dried over anhy. Na2SO4 and concentrated in vacuo to afford the title compound (449.0 mg). LC-MS: m/z 323.4 (M+H)+

後処理

  1. temperatureThe resulting mixture was then cooled
  2. custompartitioned between water and EtOAc
  3. washThe organic phase was washed with brine
  4. customdried over anhy
  5. concentrationNa2SO4 and concentrated in vacuo

出典と根拠

ORDレコード
ord-f758fce5219f408dacb7d617f7fdfb27
出典データセット
uspto-grants-2016_06
特許番号
US09365545B2

反応ノート

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