Potassium Carbonate → HCID 86632284、化合物

HRID 333125

反応式

HRID 333125 の反応式
[I:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N:8]=[C:9]=[S:10])[CH:3]=1.[NH2:11][C:12]1[S:16][C:15]([S:17]([NH2:20])(=[O:19])=[O:18])=[N:14][N:13]=1.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[I:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[S:10])[NH:11][C:12]2[S:16][C:15]([S:17]([NH2:20])(=[O:19])=[O:18])=[N:14][N:13]=2)[CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 847245-Amino-1,3,4-thiadiazole-2-sulfonamideHCID 1510833-Iodophenylisothiocyanate

生成物 1

HCID 86632284HCID 86632284、化合物収率 45%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
75 °C

実験手順

To a solution of 1-iodo-3-isothiocyanatobenzene (0.13 g, 0.50 mmol) in acetonitrile (10 mL) was added 5-amino-1,3,4-thiadiazole-2-sulfonamide (0.108 g, 0.50 mmol) and anhydrous K2CO3 (0.40 g). The mixture was stirred at 75° C. for 4 hrs. Solvent was evaporated and diluted with water. The precipitated solid was filtered and dried over vacuum to give desired compound (99 mg, 45%) as a white solid. 1H NMR (400 MHz, DMSO) δ 8.99 (brs, 1H), 8.24 (brs, 1H), 7.78 (d, J=8.0 Hz, 1H), 7.69 (t, J=1.8 Hz, 1H), 7.35 (m, 1H), 7.26 (t, J=7.8 Hz, 1H), 7.02 (s, 2H).

後処理

  1. customSolvent was evaporated
  2. additiondiluted with water
  3. filtrationThe precipitated solid was filtered
  4. customdried over vacuum

出典と根拠

ORDレコード
ord-45072d31621c4fc2840e80d11d04e0ae
出典データセット
uspto-grants-2014_11
特許番号
US08877970B2

関連ノート

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