Sodium Iodide → 1-[(4-Chlorophenyl)phenylmethyl]hexahydro-1H-1,4-diazepine

HRID 1032966노트

반응식

HRID 1032966 반응식
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([CH:6](Cl)[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[I-].[Na+].[NH:18]1[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>C(O)(C)C>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([CH:6]([N:18]2[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 68163Hexahydro-1,4-diazepineHCID 2415844-Chlorobenzhydryl chloride

생성물 1

HCID 27627031-[(4-Chlorophenyl)phenylmethyl]hexahydro-1H-1,4-diazepine

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 4-chlorobenzhydryl chloride (5.32 g, 22.4 mmol), isopropanol (80 ml) and sodium iodide (3.41 g, 22.8 mmol) was stirred at room temperature for 30 minutes. Thereto was added homopiperazine (11.2 g, 112 mmol), and the mixture was stirred at 95° C. for 18 hours. The solvent was distilled off, and the concentrate was poured into a saturated aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated. The thus-obtained crude product was used for the next reaction without purification.

후처리

  1. stirringthe mixture was stirred at 95° C. for 18 hours
  2. distillationThe solvent was distilled off
  3. additionthe concentrate was poured into a saturated aqueous solution of sodium hydrogencarbonate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated
  8. customThe thus-obtained crude product
  9. customwas used for the next reaction without purification

출처 및 근거

ORD 기록
ord-677349ed45c5437db8e0af3f48f1ebbf
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05308840

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