Triethylamine → Methanesulfonic acid 1-methoxy-piperidin-4-yl ester

HRID 2035306ノート

反応式

HRID 2035306 の反応式
[CH3:1][O:2][N:3]1[CH2:8][CH2:7][CH:6]([OH:9])[CH2:5][CH2:4]1.C(N(CC)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>C(OCC)(=O)C>[CH3:1][O:2][N:3]1[CH2:8][CH2:7][CH:6]([O:9][S:18]([CH3:17])(=[O:20])=[O:19])[CH2:5][CH2:4]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 30226061-Methoxypiperidin-4-ol

生成物 1

HCID 86663299Methanesulfonic acid 1-methoxy-piperidin-4-yl ester収率 126.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

21 g 1-Methoxy-piperidin-4-ol (from Step 1) and 19.4 g triethylamine were dissolved in 200 ml ethyl acetate, and cooled to 0° C. 15.0 g Methanesulfonyl chloride was added slowly. The resulting white suspension was stirred at 0° C. for 1 hour, then at room temperature for an additional 1 hour. Then the mixture was filtered and the solvent evaporated, yielding 34.6 g of methanesulfonic acid 1-methoxy-piperidin-4-yl ester. This material was used for the next step without further purification.

後処理

  1. waitat room temperature for an additional 1 hour
  2. filtrationThen the mixture was filtered
  3. customthe solvent evaporated

出典と根拠

ORDレコード
ord-a4235c195d2e4a28a2782dc713e599bd
出典データセット
uspto-grants-2013_11
特許番号
US08574607B2

反応ノート

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