1-(2-Amino-benzothiazol-5-yl)-3-benzoyl-thiourea → N-(2-Amino-1,3-benzothiazol-5-yl)thiourea

HRID 723953ノート

反応式

HRID 723953 の反応式
C[O-].[Na+].[NH2:4][C:5]1[S:6][C:7]2[CH:13]=[CH:12][C:11]([NH:14][C:15]([NH:17]C(=O)C3C=CC=CC=3)=[S:16])=[CH:10][C:8]=2[N:9]=1>CO>[NH2:4][C:5]1[S:6][C:7]2[CH:13]=[CH:12][C:11]([NH:14][C:15]([NH2:17])=[S:16])=[CH:10][C:8]=2[N:9]=1

参加物

4

実験手順

To a solution of anhydrous methanol (213 mL) was added sodium methoxide (1.15 g) and 1-(2-amino-benzothiazol-5-yl)-3-benzoyl-thiourea (Example 17, 3.5 g). The resulting mixture was stirred at room temperature for 3 hours. The mixture was concentrated and the residue was poured into water (300 mL). The mixture was extracted using ethyl acetate (3×200 mL). The combined organic fractions were dried over magnesium sulfate, filtered and concentrated (1.61 g, 67%). 1H-NMR (DMSO d6) δ: 9.64 (s, 1H), 760–7.37 (m, 6H), 6.96 (d, 1H, J=8.3 Hz); MS (ESI) 224.8 (M+1, 100%).

後処理

  1. concentrationThe mixture was concentrated
  2. additionthe residue was poured into water (300 mL)
  3. extractionThe mixture was extracted
  4. dry with materialThe combined organic fractions were dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated (1.61 g, 67%)

出典と根拠

ORDレコード
ord-2d147e4a4f77402cb0359c7476e5289c
出典データセット
uspto-grants-2006_11
特許番号
US07141595B2

反応ノート

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