Triethylamine → (5-Bromo-3-fluoropyridin-2-yl)methyl methanesulfonate

HRID 341041노트

반응식

HRID 341041 반응식
[Br:1][C:2]1[CH:3]=[C:4]([F:10])[C:5]([CH2:8][OH:9])=[N:6][CH:7]=1.C(N(CC)CC)C.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>ClCCl>[CH3:18][S:19]([O:9][CH2:8][C:5]1[C:4]([F:10])=[CH:3][C:2]([Br:1])=[CH:7][N:6]=1)(=[O:21])=[O:20]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 57416937(5-Bromo-3-fluoropyridin-2-yl)methanol

생성물 1

HCID 86668676(5-Bromo-3-fluoropyridin-2-yl)methyl methanesulfonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

(5-Bromo-3-fluoropyridin-2-yl)methanol (0.20 g, 0.99 mmol) was dissolved in dichloromethane (5 mL), cooled to 0° C. and treated with triethylamine (0.15 mL, 1.1 mmol, 1.1 equiv) and methanesulfonyl chloride (0.085 mL, 1.1 mmol, 1.1 equiv). After 15 minutes, the mixture was diluted with dichloromethane (100 mL) and washed once with sodium bicarbonate (20 mL, aqueous saturated) and brine (50 mL), dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

후처리

  1. washwashed once with sodium bicarbonate (20 mL, aqueous saturated) and brine (50 mL)
  2. dry with materialdried with sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-66f59257680747539b5e9c98e033cd70
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895580B2

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