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Allyl bromide → HCID 20430390, 화합물

HRID 2413113
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HRID 2413113 반응식
[Cl:1][C:2]1[C:12]2[CH2:11][CH2:10][NH:9][CH2:8][CH2:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.[CH2:13](Br)[CH:14]=[CH2:15].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[ClH:1].[CH2:15]([N:9]1[CH2:8][CH2:7][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([Cl:1])[C:12]=2[CH2:11][CH2:10]1)[CH:14]=[CH2:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 117762SK&F 101055

생성물 1

HCID 20430390HCID 20430390, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 0.52 g. of 6-chloro-2,3,4,5-tetrahydro-1H-3-benzazepine, 0.34 g. of allyl bromide, 0.6 g. of potassium carbonate and 20 ml. of 90% ethanol was stirred at room temperature for 17 hours. The mixture was filtered and the filtrate concentrated in vacuo. The residue was extracted with 35 ml. of ether and the ethereal extract treated with isopropanolic hydrogen chloride to precipitate 3-allyl-6-chloro-2,3,4,5-tetra-hydro-1H-3-benzazepine hydrochloride. Recrystallization of this salt from absolute ethanol gave 3-allyl-6-chloro-2,3,4,5-tetrahydro-1H-3-benzazepine hydrochloride having a melting point of 248°-249°.

후처리

  1. additionA mixture of 0.52 g
  2. filtrationThe mixture was filtered
  3. concentrationthe filtrate concentrated in vacuo
  4. extractionThe residue was extracted with 35 ml
  5. extractionof ether and the ethereal extract
  6. additiontreated with isopropanolic hydrogen chloride
  7. customto precipitate 3-allyl-6-chloro-2,3,4,5-tetra-hydro-1H-3-benzazepine hydrochloride
  8. customRecrystallization of this salt from absolute ethanol

출처 및 근거

ORD 기록
ord-1f97e5daafc649ff97ba3ac6d55276b7
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04496558

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