Triethylamine → 1-Adamantylmethyl methanesulfonate

HRID 605577노트

반응식

HRID 605577 반응식
[C:1]12([CH2:11][OH:12])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.C(N(CC)CC)C.[CH3:20][S:21](Cl)(=[O:23])=[O:22]>C(Cl)Cl>[CH3:20][S:21]([O:12][CH2:11][C:1]12[CH2:8][CH:7]3[CH2:6][CH:5]([CH2:4][CH:3]([CH2:9]3)[CH2:2]1)[CH2:10]2)(=[O:23])=[O:22]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 64556Tricyclo(3.3.1.1'3,7)dec-1-ylmethanol

생성물 1

HCID 28017761-Adamantylmethyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

A mixture of 3 g of adamantan-1-ylmethanol and 5 ml of triethylamine in 50 ml of DCM is cooled to 0° C., 2 ml of methanesulfonyl chloride are added dropwise, and the mixture is left to stir while allowing the temperature to return to AT. A mixture of water/ice is added to the reaction mixture, the mixture is extracted with DCM, the organic phase is dried over Na2SO4, and the solvent is evaporated off under vacuum. 2 g of the expected compound are obtained.

후처리

  1. waitthe mixture is left
  2. additionis added to the reaction mixture
  3. extractionthe mixture is extracted with DCM
  4. dry with materialthe organic phase is dried over Na2SO4
  5. customthe solvent is evaporated off under vacuum

출처 및 근거

ORD 기록
ord-27c6b6321323431a8af077abd2c5bb7f
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07915258B2

반응 노트

불러오는 중…