Carbon tetrabromide → 2H-Pyran, 2-[(12-bromododecyl)oxy]tetrahydro-

HRID 862831ノート

反応式

HRID 862831 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH:8](O)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].C(Br)(Br)(Br)[Br:22].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[Br:22][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][O:7][CH:2]1[CH2:3][CH2:4][CH2:5][CH2:6][O:1]1

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 21849359Dodecanediol monotetrahydropyranyl ether

生成物 1

HCID 110785922H-Pyran, 2-[(12-bromododecyl)oxy]tetrahydro-収率 41.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

The above-mentioned dodecanediol monotetrahydropyranyl ether (7.882 g) and 11.437 g of carbon tetrabromide were dissolved in 78 ml of dichloromethane. Triphenylphosphine (10.843 g) was added thereto under ice-cooling and the mixture was stirred at 0° C. for 5 minutes. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography to give 4.029 g of 1-bromo-12-tetrahydropyranyloxydodecane.

後処理

  1. temperatureunder ice-cooling
  2. distillationThe solvent was distilled away under reduced pressure
  3. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-569c6353de8b4f3688685e461db096ab
出典データセット
uspto-grants-1998_02
特許番号
US05719176

反応ノート

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