Sodium Carbonate → HCID 57551211、化合物

HRID 1644649ノート

反応式

HRID 1644649 の反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:12][NH2:13])=O)=[CH:5][CH:4]=1.[N:16]([C:19]1[CH:24]=[CH:23][C:22]([S:25]([NH:28][C:29]2[S:30][CH:31]=[CH:32][N:33]=2)(=[O:27])=[O:26])=[CH:21][CH:20]=1)=[C:17]=[S:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[S:30]1[CH:31]=[CH:32][N:33]=[C:29]1[NH:28][S:25]([C:22]1[CH:21]=[CH:20][C:19]([NH:16][C:17]2[S:18][C:10]([CH2:9][C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:15])([F:14])[F:1])=[CH:4][CH:5]=3)=[N:12][N:13]=2)=[CH:24][CH:23]=1)(=[O:26])=[O:27]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 44674964-isothiocyanato-N-1,3-thiazol-2-ylbenzenesulfonamideHCID 43237029HCID 43237029、化合物

生成物 1

HCID 57551211HCID 57551211、化合物収率 20%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
85 °C

実験手順

A mixture of (4-trifluoromethyl-phenyl)-acetic acid hydrazide (55 mg, 0.25 mmol, 1.5 equiv), 4-isothiocyanato-N-thiazol-2-yl-benzenesulfonamide (50 mg, 0.2 mmol, 1.0 equiv) and sodium carbonate (20 mg, 0.18 mmol, 1.1 equiv) in 1.0 mL of ethanol was heated at 85° C. After 16 h, the heterogeneous reaction mixture was concentrated in vacuo, diluted with 500 μL of acetonitrile, filtered, and purified via reverse phase HPLC. The fraction containing product was lyophilized to afford the product as an off-white solid (15 mg, 20%).

後処理

  1. concentrationthe heterogeneous reaction mixture was concentrated in vacuo
  2. additiondiluted with 500 μL of acetonitrile
  3. filtrationfiltered
  4. custompurified via reverse phase HPLC
  5. additionThe fraction containing product

出典と根拠

ORDレコード
ord-2fdb93d8572e4a72b3617c5d02932de3
出典データセット
uspto-grants-2012_02
特許番号
US08124610B2

反応ノート

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