Methanesulfonyl chloride → 1-(Diphenylmethyl)azetidin-3-yl methanesulfonate

HRID 82914

반응식

HRID 82914 반응식
[C:1]1([CH:7]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[N:8]2[CH2:11][CH:10]([OH:12])[CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>N1C=CC=CC=1>[CH3:19][S:20]([O:12][CH:10]1[CH2:11][N:8]([CH:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:9]1)(=[O:22])=[O:21]

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 3304481-(Diphenylmethyl)azetidin-3-ol

생성물 1

HCID 27587161-(Diphenylmethyl)azetidin-3-yl methanesulfonate수율 96.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
-20 °C

실험 절차

A 100 mL flask was charged with 1-diphenylmethylazetidin-3-ol (1.5 g, 6.27 mmol) and pyridine (15 mL). The solution was cooled to −20° C. and methane sulfonyl chloride (0.73 mL, 9.4 mmol) was added dropwise. The reaction mixture was stirred at −20° C. for 1 h and then left 3 days at 4° C. The solution was poured on ice and the resulting precipitate was filtered, washed 3 times with H2O and 3 times with pentane. The solid was dried under reduced pressure to give the title compound (1.92 g, 96%) as a white solid.

후처리

  1. waitleft 3 days at 4° C
  2. additionThe solution was poured on ice
  3. filtrationthe resulting precipitate was filtered
  4. washwashed 3 times with H2O and 3 times with pentane
  5. customThe solid was dried under reduced pressure

출처 및 근거

ORD 기록
ord-9a1bde83ffcd4def8f7bb5e71f141f7a
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846711B2

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