Triethylamine → HCID 13638465, 화합물

HRID 2169194노트

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HRID 2169194 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 13638465HCID 13638465, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2ea9144fece349eea69f4b5959898184
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09045486B2

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