Triethylamine → 3-Ethynyl-1-(propane-2-sulfonyl)piperidine

HRID 1521935

反応式

HRID 1521935 の反応式
[C:1]([CH:3]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4]1)#[CH:2].C(N(CC)CC)C.[CH3:16][CH:17]([S:19](Cl)(=[O:21])=[O:20])[CH3:18]>ClCCl>[C:1]([CH:3]1[CH2:8][CH2:7][CH2:6][N:5]([S:19]([CH:17]([CH3:18])[CH3:16])(=[O:21])=[O:20])[CH2:4]1)#[CH:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 824082-Propanesulfonyl chlorideHCID 219638583-Ethynylpiperidine

生成物 1

HCID 904115943-Ethynyl-1-(propane-2-sulfonyl)piperidine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of Example 10A (500 mg, 4.58 mmol) in dichloromethane (10 mL) was added triethylamine (2.55 mL, 18.32 mmol) followed by propane-2-sulfonyl chloride (1.306 g, 9.16 mmol) and the mixture was stirred for 3 hours. The mixture was concentrated and the residue was dissolved in ethyl acetate, washed with water and brine, dried over anhydrous sodium sulfate, filtered, and concentrated. Purification by column chromatography (silica gel, 30% ethyl acetate in hexane) afforded the title compound. LCMS: 216.2 (M+H-Boc)+.

後処理

  1. concentrationThe mixture was concentrated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customPurification by column chromatography (silica gel, 30% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-b8806f98aaf7449fae4f26dfec97ece2
出典データセット
uspto-grants-2015_07
特許番号
US09073922B2

関連ノート

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