2-Chloroethyl chloroformate → 5-Methyl-1,4-oxazepane hydrochloride

HRID 515445노트

반응식

HRID 515445 반응식
C([N:8]1[CH:14]([CH3:15])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:16]C(OCCCl)=O>ClCCCl>[ClH:16].[CH3:15][CH:14]1[CH2:13][CH2:12][O:11][CH2:10][CH2:9][NH:8]1

참가 물질

4

반응물 2

HCID 123052-Chloroethyl chloroformateHCID 667187904-Benzyl-5-methyl-[1,4]oxazepane

생성물 1

HCID 667186395-Methyl-1,4-oxazepane hydrochloride수율 78.6%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid.

후처리

  1. temperatureThe mixture was refluxed for 10 hours
  2. concentrationconcentrated
  3. dissolutionThe resulting residue was dissolved in methanol (5 mL)
  4. temperaturethe solution was refluxed for one hour
  5. concentrationAfter concentration
  6. customthe residual material was triturated
  7. washwashed with ethyl acetate
  8. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-337a7b879283470cba51f99f8306b20f
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09108957B2

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