Triethylamine → 1-Methylpiperidin-4-yl methanesulfonate

HRID 64056

反応式

HRID 64056 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([OH:8])[CH2:4][CH2:3]1.CCN(CC)CC.[CH3:16][S:17](Cl)(=[O:19])=[O:18]>C(Cl)Cl>[CH3:16][S:17]([O:8][CH:5]1[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1)(=[O:19])=[O:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 660484-Piperidinol, 1-methyl-

生成物 1

HCID 41906811-Methylpiperidin-4-yl methanesulfonate収率 99.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-Methylpiperidin-4-ol (4 g, 34.7 mmol) was dissolved in CH2Cl2 (70 ml) at 0° C. followed by the addition of Et3N (10 ml, 69.4 mmol, 2 eq.) and methanesulfonyl chloride (2.7 ml, 34.7 mmol, 1 eq.). The mixture was stirred at RT for 3 h and quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to afford the crude product (6.7 g).

後処理

  1. customquenched
  2. extractionextracted as in Intermediate Example 5(a)
  3. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-95d2427a2ebc434081e05472c18fdde3
出典データセット
uspto-grants-2016_09
特許番号
US09447091B2

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