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Dichloromethane → 4-Allyl-7,7-diphenyl-1,4-oxazepane hydrochloride

HRID 596165
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HRID 596165 반응식
[C:1]1([C:7]2([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[O:13][CH2:12][CH2:11][NH:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:20](Br)[CH:21]=[CH2:22].C(=O)(O)[O-].[Na+].C(Cl)[Cl:30]>>[ClH:30].[CH2:22]([N:10]1[CH2:9][CH2:8][C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[O:13][CH2:12][CH2:11]1)[CH:21]=[CH2:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6344DichloromethaneHCID 7841Allyl bromideHCID 516892Sodium BicarbonateHCID 203266297,7-Diphenyl-1,4-oxazepane

생성물 1

HCID 214507464-Allyl-7,7-diphenyl-1,4-oxazepane hydrochloride

실험 절차

To the stirred solution of 5.06 g of 7,7-diphenyl-hexahydro-1,4-oxazepine in 50 ml of methylene chloride, 2.6 g of allyl bromide are added, followed by 40 ml of 10% aqueous sodium bicarbonate and the mixture is stirred for 24 hours at room temperature. The organic layer is separated, washed with water, dried, filtered and evaporated. The residue is taken up in acetone, the solution acidified with hydrogen chloride in acetone and diluted with diethyl ether, to yield the 4-allyl-7,7-diphenyl-hexahydro-1,4-oxazepine hydrochloride melting at 246° to 247°.

후처리

  1. customThe organic layer is separated
  2. washwashed with water
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. additiondiluted with diethyl ether

출처 및 근거

ORD 기록
ord-66ea9860a23943669ddd612cac5b6dc2
출처 데이터셋
uspto-grants-1977_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04010166

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