1-Chloro-2-isothiocyanatobenzene → HCID 178527962、化合物

HRID 334513

反応式

HRID 334513 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]=[C:9]=[S:10].[Cl:11][C:12]1[CH:17]=[C:16]([C:18]([NH:20][NH2:21])=O)[CH:15]=[CH:14][N:13]=1>CN(C=O)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:18]([C:16]2[CH:15]=[CH:14][N:13]=[C:12]([Cl:11])[CH:17]=2)=[N:20][N:21]=[C:9]1[SH:10]

参加物

4

反応物 2

HCID 1231711-Chloro-2-isothiocyanatobenzeneHCID 2362062-Chloropyridine-4-carbohydrazide

生成物 1

HCID 178527962HCID 178527962、化合物収率 571%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-chloro-2-isothiocyanatobenzene 1 (0.4 g, 2.33 mmol) and 2-chloropyridine-4-carbohydrazide 11 (0.4 g, 2.33 mmol) in DMF was stirred at ambient temperature for 18 hours, concentrated to dryness, and 20 mL of 10% K2CO3 (aq.) was added. The resulting mixture was stirred under reflux for 6 hours. The clear solution was cooled to ambient temperature, washed with ether, and acidified with 1N HCl. The solid was collected, washed with H2O and ether, and dried to afford compound 13 (4.3 g). Yield: 86%.

後処理

  1. concentrationconcentrated to dryness, and 20 mL of 10% K2CO3 (aq.)
  2. additionwas added
  3. stirringThe resulting mixture was stirred
  4. temperatureunder reflux for 6 hours
  5. temperatureThe clear solution was cooled to ambient temperature
  6. washwashed with ether
  7. customThe solid was collected
  8. washwashed with H2O and ether
  9. customdried

出典と根拠

ORDレコード
ord-a9f247e8e7a24f389e5e7a56d4ea3ef2
出典データセット
uspto-grants-2014_11
特許番号
US08883827B2

関連ノート

読み込み中…