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

HRID 341041ノート

反応式

HRID 341041 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-66f59257680747539b5e9c98e033cd70
出典データセット
uspto-grants-2014_11
特許番号
US08895580B2

反応ノート

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