Triethylamine → 2-(N-tert-Butoxycarbonylpiperidin-2-yl)ethyl methanesulfonate

HRID 1437220ノート

反応式

HRID 1437220 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH:9]1[CH2:14][CH2:15][OH:16])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(N(CC)CC)C.[CH3:24][S:25](Cl)(=[O:27])=[O:26]>C(Cl)Cl>[CH3:24][S:25]([O:16][CH2:15][CH2:14][CH:9]1[CH2:10][CH2:11][CH2:12][CH2:13][N:8]1[C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])(=[O:27])=[O:26]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 5103438Tert-butyl 2-(2-hydroxyethyl)piperidine-1-carboxylate

生成物 1

HCID 230901662-(N-tert-Butoxycarbonylpiperidin-2-yl)ethyl methanesulfonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

2-(2-Hydroxyethyl)piperidine-1-carboxylic acid tert-butyl ester (229 mg) obtained from Referential Example 77 and triethylamine (209 μL) were dissolved in methylene chloride (5 mL) To the resultant solution, methanesulfonyl chloride (116 μL) was added at room temperature, followed by stirring for 30 minutes. The residue obtained by removal through evaporation of the reaction solvent under reduced pressure was partitioned between water and methylene chloride. The organic layer was sequentially washed with water and saturated brine, and then dried over sodium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, to thereby give the title compound in the form of crystals (288 mg, 93%).

後処理

  1. additionwas added at room temperature
  2. customThe residue obtained by removal through evaporation of the reaction solvent under reduced pressure
  3. customwas partitioned between water and methylene chloride
  4. washThe organic layer was sequentially washed with water and saturated brine
  5. dry with materialdried over sodium sulfate anhydrate
  6. filtrationfollowed by filtration
  7. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-cb72dbc54cee452db7a6cc4c5b704a6e
出典データセット
uspto-grants-2009_11
特許番号
US07622471B2

反応ノート

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