Triethylamine → (1-Methylpiperidin-2-yl)methyl methanesulfonate

HRID 227369

반응식

HRID 227369 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][OH:9].C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>O1CCCC1>[CH3:17][S:18]([O:9][CH2:8][CH:3]1[CH2:4][CH2:5][CH2:6][CH2:7][N:2]1[CH3:1])(=[O:20])=[O:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 893941-Methyl-2-piperidinemethanol

생성물 1

HCID 44627021(1-Methylpiperidin-2-yl)methyl methanesulfonate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

To a solution of 1-methyl-2-piperidine-methanol (Aldrich, 0.27 mL, 2.1 mmol) in 10 mL tetrahydrofuran (THF) at 0° C. was added triethylamine (0.87 mL, 6.22 mmol) followed by methanesulfonyl chloride (0.24 mL, 3.1 mmol). The mixture was stirred at 0° C. for 10 min then the ice-bath was removed and the reaction mixture was stirred at 23° C. for an additional 1.5 h. The reaction mixture was filtered though Celite with THF and concentrated under reduced pressure. This crude material was used directly in the next reaction.

후처리

  1. customthe ice-bath was removed
  2. stirringthe reaction mixture was stirred at 23° C. for an additional 1.5 h
  3. filtrationThe reaction mixture was filtered though Celite with THF
  4. concentrationconcentrated under reduced pressure
  5. customThis crude material was used directly in the next reaction

출처 및 근거

ORD 기록
ord-a17f828435f94eff96c61b543cf3d75e
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07560481B2

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