Water → Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

HRID 1853372ノート

反応式

HRID 1853372 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:12][CH2:11][CH:10]([OH:13])[CH2:9][CH2:8]1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23].O>ClCCl>[N:1]1[CH:6]=[CH:5][CH:4]=[N:3][C:2]=1[N:7]1[CH2:8][CH2:9][CH:10]([O:13][S:22]([CH3:21])(=[O:24])=[O:23])[CH2:11][CH2:12]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 202340981-(Pyrimidin-2-yl)piperidin-4-ol

生成物 1

HCID 86673125Methanesulfonic acid 1-pyrimidin-2-yl-piperidin-4-yl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a cooled solution of 1-Pyrimidin-2-yl-piperidin-4-ol (WO2008/8895 A1), (100 mg; 0.55 mmol) and triethylamine (233 μL, 1.67 mmol) in dry dichloromethane (1 mL), was added methanesulfonyl chloride (52 μL, 0.67 mmol). The reaction mixture was stirred at room temperature for 5 hours. Water was added. After extraction with dichloromethane, the combined organic extracts were dried over sodium sulfate and concentrated to afford a crude product that was used in the next step without further purification.

後処理

  1. extractionAfter extraction with dichloromethane
  2. dry with materialthe combined organic extracts were dried over sodium sulfate
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-eaf8a611c1f04dc9a9b81630d20d065e
出典データセット
uspto-grants-2015_02
特許番号
US08962627B2

反応ノート

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