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Ethyl chloroformate → HCID 20326661, 화합물

HRID 372793
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HRID 372793 반응식
C([N:8]1[CH2:14][CH2:13][C:12]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.Cl[C:28]([O:30][CH2:31][CH3:32])=[O:29]>C(Cl)Cl>[C:28]([N:8]1[CH2:14][CH2:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[O:11][CH2:10][CH2:9]1)([O:30][CH2:31][CH3:32])=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10928Ethyl chloroformateHCID 203266454-Benzyl-7,7-diphenyl-1,4-oxazepane

생성물 1

HCID 20326661HCID 20326661, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To the solution of 30.25 g of 4-benzyl-7,7-diphenylhexahydro-1,4-oxazepine in 300 ml of methylene chloride, that of 10.4 g of ethyl chloroformate in 100 ml of methylene chloride is added dropwise while stirring. After 30 minutes the mixture is allowed to warm up to room temperature and stirred for 15 hours. It is successively washed twice with 50 ml of N hydrochloric acid, 50 ml of N aqueous sodium hydroxide and 50 ml of saturated sodium chloride each, dried, filtered and evaporated. The residue is recrystallized from hexane, to yield the 4-carbethoxy-7,7-diphenylhexahydro-1,4-oxazepine melting at 122° to 123°.

후처리

  1. stirringstirred for 15 hours
  2. washIt is successively washed twice with 50 ml of N hydrochloric acid, 50 ml of N aqueous sodium hydroxide and 50 ml of saturated sodium chloride each,
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue is recrystallized from hexane

출처 및 근거

ORD 기록
ord-19a0034140db44659b7469159978bdf2
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04092330

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