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Ammonium Chloride → beta(R)-benzyloxy-alpha(RS)-phenyl-1,4-dioxaspiro[4,5]decane-2(R)-ethanol

HRID 440109
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HRID 440109 반응식
[CH2:1]([O:8][C@@H:9]([C@H:12]1[CH2:16][O:15][C:14]2([CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[O:13]1)[CH:10]=[O:11])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:22]1([Mg]Cl)[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.[Cl-].[NH4+]>C(OCC)C.O1CCCC1>[CH2:1]([O:8][C@@H:9]([C@H:12]1[CH2:16][O:15][C:14]2([CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[O:13]1)[CH:10]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)[OH:11])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 22856132alpha(S)-benzyloxy-1,4-dioxaspiro[4,5]decane-2(R)-acetaldehydeHCID 178478979HCID 178478979, 화합물

생성물 1

HCID 22856134beta(R)-benzyloxy-alpha(RS)-phenyl-1,4-dioxaspiro[4,5]decane-2(R)-ethanol

시약·촉매·용매 2

HCID 3283Diethyl Ether용매
HCID 8028
Tetrahydrofuran
용매

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온도
-5 °C

실험 절차

A solution of 4.30 g (0.015 mmol) of α(S)-benzyloxy-1,4-dioxaspiro[4,5]decane-2(R)-acetaldehyde in 50 ml of anhydrous diethyl ether was cooled to -8° C. and 15 ml of a 2M solution of phenylmagnesium chloride in tetrahydrofuran were added dropwise over a period of 1 hour. The mixture was stirred at -5° C. for 2 hours, then allowed to warm to room temperature and poured into 50 ml of 10% ammonium chloride solution. The mixture was extracted twice with 100 ml of ethyl acetate each time. The ethyl acetate extracts were dried over anhydrous magnesium sulphate and evaporated. The residue was subjected to flash chromatography on silica gel using 5% methanol in dichloromethane for the elution. There were obtained 2.47 g of β(R)-benzyloxy-α(RS)-phenyl-1,4-dioxaspiro[4,5]decane-2(R)-ethanol in the form of a colourless gum; MS (C.I.): m/e 369 [M+H]+.

후처리

  1. temperatureto warm to room temperature
  2. extractionThe mixture was extracted twice with 100 ml of ethyl acetate each time
  3. dry with materialThe ethyl acetate extracts were dried over anhydrous magnesium sulphate
  4. customevaporated
  5. washThe residue was subjected to flash chromatography on silica gel using 5% methanol in dichloromethane for the elution

출처 및 근거

ORD 기록
ord-00a3942df72e41fd92d745486a516d85
출처 데이터셋
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05516913

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