Triethylamine → Tert-butyl (4-{2-[(methylsulfonyl)oxy]ethyl}phenoxy)acetate

HRID 898889

반응식

HRID 898889 반응식
[OH:1][CH2:2][CH2:3][C:4]1[CH:18]=[CH:17][C:7]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])=[CH:6][CH:5]=1.C(N(CC)CC)C.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>C(Cl)Cl>[CH3:26][S:27]([O:1][CH2:2][CH2:3][C:4]1[CH:5]=[CH:6][C:7]([O:8][CH2:9][C:10]([O:12][C:13]([CH3:15])([CH3:14])[CH3:16])=[O:11])=[CH:17][CH:18]=1)(=[O:29])=[O:28]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 23119602Tert-butyl [4-(2-hydroxyethyl)phenoxy]acetate

생성물 1

HCID 86600965Tert-butyl (4-{2-[(methylsulfonyl)oxy]ethyl}phenoxy)acetate수율 95.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
-10 °C

실험 절차

Tert-butyl [4-(2-hydroxyethyl)phenoxy]acetate (6.000 g, 23.781 mmol) and triethylamine (9.9 ml, 71.341 mmol) were dissolved in DCM. The mixture was cooled to −10° C. and methanesulfonyl chloride (2.8 ml, 35.671 mmol) was added dropwise to the mixture. The reaction mixture was allowed to reach room temperature and was stirred for 16 hours. The mixture was diluted with DCM. The organic layer was washed with water, brine and 0.3M KHSO4, dried with MgSO4, and evaporated under reduced pressure. Obtained 7.5 g of light-yellow crystals (yield 95.5%).

후처리

  1. customto reach room temperature
  2. washThe organic layer was washed with water, brine and 0.3M KHSO4
  3. dry with materialdried with MgSO4
  4. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-645b4593cacc44a79a13e29e22ae538e
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07351858B2

연결된 노트

불러오는 중…