Triethylamine → HCID 66920960, 화합물

HRID 2066335노트

반응식

HRID 2066335 반응식
Cl[S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3].Br[CH:9]([OH:11])[CH3:10].[CH3:12][Si:13]([CH:16]([NH2:21])[Si:17]([CH3:20])([CH3:19])[CH3:18])([CH3:15])[CH3:14].C(N(CC)CC)C>ClCCl>[CH3:12][Si:13]([CH:16]([NH:21][S:2]([N:5]1[CH2:10][CH2:9][O:11][C:6]1=[O:7])(=[O:4])=[O:3])[Si:17]([CH3:20])([CH3:19])[CH3:18])([CH3:15])[CH3:14]

참가 물질

6

반응물 4

HCID 8471Triethylamine2회HCID 70918Chlorosulfonyl isocyanateHCID 10997564Bis(trimethylsilyl)methylamineHCID 14202443Ethanol, 1-bromo-

생성물 1

HCID 66920960HCID 66920960, 화합물수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매4회

반응 조건

온도
0 °C

실험 절차

To 2.18 ml of chlorosulfonyl isocyanate in 10 ml of dichloromethane is added dropwise, at 0° C., a solution of 1.77 ml of bromoethanol in 10 ml of dichloromethane. The reaction medium is stirred for 10 minutes at 0° C. and then added dropwise to a solution of 4.38 grams of bis(trimethylsilyl)methylamine and 3.51 ml of triethylamine in 40 ml of dichloromethane at 0° C. After warming to 20° C. and stirring for 4 hours, the reaction mixture is cooled to 0° C. and 10.5 ml of triethylamine are then added dropwise. The reaction mixture is then stirred overnight at room temperature. It is then diluted with dichloromethane and washed 3 times with dilute hydrochloric acid. The organic phase is then washed once with saturated aqueous NaCl solution and then dried over sodium sulfate and concentrated under reduced pressure to give a white solid, 2-oxooxazolidine-3-sulfonic acid [bis(trimethylsilanyl)methyl]amide (65% yield).

후처리

  1. temperatureAfter warming to 20° C.
  2. stirringstirring for 4 hours
  3. temperaturethe reaction mixture is cooled to 0° C.
  4. stirringThe reaction mixture is then stirred overnight at room temperature
  5. washwashed 3 times with dilute hydrochloric acid
  6. washThe organic phase is then washed once with saturated aqueous NaCl solution
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-88cdd496e0ba4fde8d1557f44031cc6f
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293256B2

반응 노트

불러오는 중…