Water → (2-Oxo-1-phenylpiperidin-4-yl)methyl methanesulfonate

HRID 341051ノート

反応式

HRID 341051 の反応式
[OH:1][CH2:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5](=[O:15])[CH2:4]1.C(N(CC)CC)C.[CH3:23][S:24](Cl)(=[O:26])=[O:25].O>ClCCl>[CH3:23][S:24]([O:1][CH2:2][CH:3]1[CH2:8][CH2:7][N:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:5](=[O:15])[CH2:4]1)(=[O:26])=[O:25]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 154282234-(Hydroxymethyl)-1-phenylpiperidin-2-one

生成物 1

HCID 86668677(2-Oxo-1-phenylpiperidin-4-yl)methyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

4-(Hydroxymethyl)-1-phenylpiperidin-2-one (0.27 g, 1.3 mmol) was dissolved in dichloromethane (15 mL), cooled to 0° C. and treated with triethylamine (1.0 mL, 7.2 mmol, 5.5 equiv). To the mixture was added methanesulfonyl chloride (0.10 mL, 1.3 mmol, 1 equiv), the mixture was warmed to ambient temperature and stirred for an additional 15 hours. The mixture was poured into water (25 mL) and extracted with dichloromethane (2×20 mL). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

後処理

  1. temperaturethe mixture was warmed to ambient temperature
  2. extractionextracted with dichloromethane (2×20 mL)
  3. dry with materialThe combined organic extracts were dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-78f78218f2f74335aee45edbbba99cab
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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