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Methanol → trans-Decahydroisoquinoline

HRID 904757
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HRID 904757 반응식
C[N:2]1[CH2:11][CH2:10][C@@:9]2(C3C=CC=C(OC)C=3)[C@@H:4]([CH2:5][CH2:6][CH2:7][CH2:8]2)[CH2:3]1.B(Br)(Br)Br.CO>C(Cl)Cl>[CH2:3]1[C@H:4]2[C@@H:9]([CH2:8][CH2:7][CH2:6][CH2:5]2)[CH2:10][CH2:11][NH:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 25134Boron tribromideHCID 13107983(4aR,8aR)-4a-(3-Methoxyphenyl)-2-methyldecahydroisoquinoline

생성물 1

HCID 11083964trans-Decahydroisoquinoline

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 800 mg of N-methyl-4a-(m-methoxyphenyl)-trans-decahydroisoquinoline (3.09 mmoles) in 30 ml of methylene chloride was added in portions to an ice-cold solution of 0.59 ml (1.55 g, 6.18 mmoles) of boron tribromide in 15 ml of methylene chloride. The solution, protected under nitrogen, was kept overnight at 25° C. Methanol (5 ml) was then added and the solution evaporated. The residue was treated with 15 ml of 5 N aqueous sodium hydroxide and the mixture stirred for 15 minutes. Ether (50 ml) was added and the bilayer mixture stirred for 2 hours. The aqueous and ether layers were finally separated and the aqueous portion saturated with carbon dioxide. The resulting solid precipitate was extracted with ether and the extract concentrated to give 680 mg of N-methyl-4a-(m-hydroxyphenyl)-trans-decahydroisoquinoline, mp 195°-205° C.

후처리

  1. customthe solution evaporated
  2. additionThe residue was treated with 15 ml of 5 N aqueous sodium hydroxide
  3. additionEther (50 ml) was added
  4. stirringthe bilayer mixture stirred for 2 hours
  5. customThe aqueous and ether layers were finally separated
  6. extractionThe resulting solid precipitate was extracted with ether
  7. concentrationthe extract concentrated
  8. customto give 680 mg of N-methyl-4a-(m-hydroxyphenyl)-trans-decahydroisoquinoline, mp 195°-205° C.

출처 및 근거

ORD 기록
ord-a17c55ec2dbd4b41b596bd72eeee25f8
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04419517

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