1-Chloro-2-isothiocyanatobenzene → HCID 178527962, 화합물

HRID 334513

반응식

HRID 334513 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178527962HCID 178527962, 화합물수율 571%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-a9f247e8e7a24f389e5e7a56d4ea3ef2
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883827B2

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