Triethylamine → Methanesulfonic acid 2-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenoxy]-ethyl ester

HRID 403488ノート

反応式

HRID 403488 の反応式
[CH2:1]([C:3]1[C:13]([CH2:14][C:15]2[CH:24]=[CH:23][C:18]([O:19][CH2:20][CH2:21][OH:22])=[CH:17][CH:16]=2)=[C:6]2[N:7]=[C:8]([CH3:12])[CH:9]=[C:10]([CH3:11])[N:5]2[N:4]=1)[CH3:2].[CH3:25][S:26](Cl)(=[O:28])=[O:27].CCN(CC)CC>>[CH2:1]([C:3]1[C:13]([CH2:14][C:15]2[CH:16]=[CH:17][C:18]([O:19][CH2:20][CH2:21][O:22][S:26]([CH3:25])(=[O:28])=[O:27])=[CH:23][CH:24]=2)=[C:6]2[N:7]=[C:8]([CH3:12])[CH:9]=[C:10]([CH3:11])[N:5]2[N:4]=1)[CH3:2]

参加物

4

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 683794832-[4-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenoxy]-ethanol

生成物 1

HCID 86671752Methanesulfonic acid 2-[4-(2-ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenoxy]-ethyl ester

実験手順

A mixture of 2-[4-(2-Ethyl-5,7-dimethyl-pyrazolo[1,5-a]pyrimidin-3-ylmethyl)-phenoxy]-ethanol (10) (200 mg, 0.62 mmol), methanesulfonyl chloride (0.05 ml, 0.62 mmol) and Et3N (0.09 ml, 0.62 mmol) was stirred at room temperature for 2 h. Then the reaction was quenched by addition of CH2Cl2 and water. The organic layer was then extracted with water and NaCl-solution, dried over Na2 SO4 and evaporated. The crude product was used in the next step without purification.

後処理

  1. customThen the reaction was quenched by addition of CH2Cl2 and water
  2. extractionThe organic layer was then extracted with water and NaCl-solution
  3. customdried over Na2 SO4
  4. customevaporated
  5. customThe crude product was used in the next step without purification

出典と根拠

ORDレコード
ord-b0323163defe44a99204cba07a3a8913
出典データセット
uspto-grants-2014_06
特許番号
US08748435B2

反応ノート

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