Hexamethylphosphoramide → HCID 86681263、化合物

HRID 336589

反応式

HRID 336589 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 86681263HCID 86681263、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
250 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-32df780e4a2c43c38b62dc29c3a6c1f6
出典データセット
uspto-grants-2014_11
特許番号
US08889675B2

関連ノート

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