Hexamethylphosphoramide → HCID 86681263, 화합물

HRID 336589

반응식

HRID 336589 반응식
[Br:1][C:2]1[C:3]([CH3:9])=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.Br[C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][CH:13]([CH2:14]3)[CH2:12]1)[CH2:18]2.CN(C)P(N(C)C)(N(C)C)=O>C(OCC)C>[Br:1][C:2]1[C:3]([CH3:9])=[C:4]([CH:5]=[CH:6][CH:7]=1)[O:8][C:11]12[CH2:20][CH:15]3[CH2:16][CH:17]([CH2:19][CH:13]([CH2:14]3)[CH2:12]1)[CH2:18]2

참가 물질

5

반응물 3

HCID 12679HexamethylphosphoramideHCID 791061-BromoadamantaneHCID 111714303-Bromo-2-methylphenol

생성물 1

HCID 86681263HCID 86681263, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
250 °C

실험 절차

3-Bromo-2-methylphenol (1000 mg) and 1-bromoadamantane (2013 mg) were added to hexamethylphosphoramide (8 mL) and the mixture was heated in a microwave reactor (Biotage) at 250° C. for 35 minutes. The solution was taken up in diethyl ether, washed with water two times, washed with brine, dried on anhydrous sodium sulfate, filtered, and concentrated. The crude material was purified by flash column chromatography on silica gel using 2% ethyl acetate (hexanes) increasing to 5% ethyl acetate (hexanes) to yield the title compound.

후처리

  1. washwashed with water two times
  2. washwashed with brine
  3. dry with materialdried on anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe crude material was purified by flash column chromatography on silica gel using 2% ethyl acetate (hexanes)
  7. temperatureincreasing to 5% ethyl acetate (hexanes)

출처 및 근거

ORD 기록
ord-32df780e4a2c43c38b62dc29c3a6c1f6
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889675B2

연결된 노트

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