Triethylamine → HCID 13638465、化合物

HRID 2169194ノート

反応式

HRID 2169194 の反応式
[CH3:1][C:2]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:5])[CH2:3][OH:4].C(N(CC)CC)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>ClCCl>[CH3:19][S:20]([O:4][CH2:3][C:2]([CH3:1])([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[CH3:5])(=[O:22])=[O:21]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 219535beta,beta-Dimethylbenzeneethanol

生成物 1

HCID 13638465HCID 13638465、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

2-Methyl-2-phenylpropan-1-ol (51) (8.5 g, 56.6 mmol, Eq: 1.00) was stirred in dichloromethane (90.4 ml) at 0° C., triethylamine (6.87 g, 9.46 ml, 67.9 mmol, Eq: 1.2) and then methanesulfonyl chloride (7.13 g, 4.82 ml, 62.2 mmol, Eq: 1.1) were added over 3 minutes. The reaction mixture was stirred at 0° C. for 30 minutes, removed from the ice bat h and allowed to warm to room temperature and stirred for 15 hours. The reaction mixture was diluted with dichloromethane, washed with water, saturated sodium bicarbonate, and brine, and dried with magnesium sulfate. The solvent was removed on a rotary evaporator to give 2-methyl-2-phenylpropyl methanesulfonate (52) as a clear oil, (12.0 g, 93%).

後処理

  1. customremoved from the ice bat h
  2. temperatureto warm to room temperature
  3. stirringstirred for 15 hours
  4. additionThe reaction mixture was diluted with dichloromethane
  5. washwashed with water, saturated sodium bicarbonate, and brine
  6. dry with materialdried with magnesium sulfate
  7. customThe solvent was removed on a rotary evaporator

出典と根拠

ORDレコード
ord-2ea9144fece349eea69f4b5959898184
出典データセット
uspto-grants-2015_06
特許番号
US09045486B2

反応ノート

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