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Acetic Anhydride → HCID 11417634, 화합물

HRID 1951313
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HRID 1951313 반응식
[C:1](OC(=O)C)(=[O:3])[CH3:2].Cl.[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]2[CH2:15][C@H:16]3[NH:27][CH2:26][CH2:25][C@@:22]4([C:23]=2[CH:24]=1)[C@H:17]3[CH2:18][CH2:19][CH2:20][CH2:21]4.C(N(CC)CC)C>>[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]2[CH2:15][C@H:16]3[N:27]([C:1](=[O:3])[CH3:2])[CH2:26][CH2:25][C@@:22]4([C:23]=2[CH:24]=1)[C@H:17]3[CH2:18][CH2:19][CH2:20][CH2:21]4
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참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 115655693-Methoxymorphinan hydrochloride (nor-de xtromethorphan

생성물 1

HCID 11417634HCID 11417634, 화합물수율 81.9%

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온도
60 °C

실험 절차

Acetic anhydride (3.14 g, 30.76 mmol) was added to a solution of (+)-3-methoxy-morphinan hydrochloride (1.5 g, 5.1 mmol) in TI-IF (30 ml) and triethylamine (8.7 g, 85.98 mmol) in the presence of nitrogen. The resulting solution was heated at 60° C. for 15 hr. The reaction mixture was cooled to room temperature and evaporated under vacuum. The residue was dissolved in methylene chloride (50 ml), washed with water (40 ml×2) and dried (MgSO4). Evaporation of the dried solution gave a tan viscous oil (1.25 g, 81% yield); ms (ESI+): m/z 300 (M+1).

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customevaporated under vacuum
  3. dissolutionThe residue was dissolved in methylene chloride (50 ml)
  4. washwashed with water (40 ml×2)
  5. dry with materialdried (MgSO4)
  6. customEvaporation of the dried solution

출처 및 근거

ORD 기록
ord-5948bd3e91524b5c9b54b5117ec13050
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404706B2

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