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

HRID 514875ノート

反応式

HRID 514875 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-0e298d04b4dd4482a96aa25d755a82b0
出典データセット
uspto-grants-2015_08
特許番号
US09108921B2

反応ノート

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