Sodium Carbonate → 6-(2,4-Dimethylphenyl)pyridazine-3-thiol

HRID 868744ノート

反応式

HRID 868744 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([CH3:14])=[CH:10][C:9]=2[CH3:15])=[CH:6][CH:7]=1.NC(N)=[S:18].C([O-])([O-])=O.[Na+].[Na+]>CCO>[CH3:15][C:9]1[CH:10]=[C:11]([CH3:14])[CH:12]=[CH:13][C:8]=1[C:5]1[CH:6]=[CH:7][C:2](=[S:18])[NH:3][N:4]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 2723790ThioureaHCID 123687643-Chloro-6-(2,4-dimethylphenyl)pyridazine

生成物 1

HCID 125621006-(2,4-Dimethylphenyl)pyridazine-3-thiol収率 83.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

3-chloro-6-(2,4-dimethylphenyl)pyridazine (example 13b) (1.36 g) was refluxed with thiourea (473 mg, 6.2 mmol) in EtOH (25 mL) for 5 hrs. The mixture was evaporated, and water (45 mL) was added to the residue, followed by Na2CO3 (318 mg, 3 mmol). The precipitate that formed was collected by filtration, washed with diethylether and dried to give 6-(2,4-Dimethylphenyl)pyridazine-3(2H)-thione (1.12 g, 52%). 1H NMR (300 MHz, dMSO): δ 2.29 (s, 3H), 2.32 (s, 3H), 7.12-7.30 (m, 2H), 7.29-7.31 (d, 1H), 7.46-7.49 (d, 1H), 7.65-7.68 (dd, 1H); MS (M+H, 217).

後処理

  1. customThe mixture was evaporated
  2. additionwater (45 mL) was added to the residue
  3. customThe precipitate that formed
  4. filtrationwas collected by filtration
  5. washwashed with diethylether
  6. customdried

出典と根拠

ORDレコード
ord-921e90b7b806411aa18f29e0697c784b
出典データセット
uspto-grants-2015_03
特許番号
US08968708B2

反応ノート

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