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Carbon tetrabromide → HCID 23064812, 화합물

HRID 735403
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HRID 735403 반응식
Br[C:2]([Br:5])(Br)Br.[CH:6]12[O:14][CH:9]([CH:10](CO)[CH2:11]1)[CH:8]=[CH:7]2.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[CH:9]12[O:14][CH:6]([CH:11]([CH2:2][Br:5])[CH2:10]1)[CH:7]=[CH:8]2
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참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 2650927-Oxabicyclo[2.2.1]hept-5-en-2-ylmethanol

생성물 1

HCID 23064812HCID 23064812, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Tetrabromomethane (1.161 g, 3.50 mmol) was added to a solution of 7-oxanorborn-2-en-5-ylmethanol (0.305 g, 2.50 mmol, from Example 2) in CH2Cl2 (12.5 ml). The solution was cooled to 0° C. and admixed with triphenylphosphine (1.836 g, 7 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 12 h. The solvent was removed under reduced pressure and the remaining solid was taken up in cyclohexane. The crude product was purified by flash chromatography (using a 98:2 mixture of cyclohexane and ethyl acetate). 0.3 g (59% of theory) of the pure product were obtained. The product was stored under cool conditions with the exclusion of light.

후처리

  1. temperatureto warm to room temperature
  2. customThe solvent was removed under reduced pressure
  3. customThe crude product was purified by flash chromatography (
  4. additiona 98:2 mixture of cyclohexane and ethyl acetate)
  5. custom0.3 g (59% of theory) of the pure product were obtained

출처 및 근거

ORD 기록
ord-afc0d1d530544a1a8b3b9d59f999295f
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592498B2

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