Methanesulfonyl chloride → HCID 86702165、化合物

HRID 1776246ノート

反応式

HRID 1776246 の反応式
[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH:5]([NH2:9])[CH2:4]1.[CH3:10][S:11](Cl)(=[O:13])=[O:12]>N1C=CC=CC=1>[CH3:1][O:2][CH:3]1[CH2:8][CH2:7][CH2:6][CH:5]([NH:9][S:11]([CH3:10])(=[O:13])=[O:12])[CH2:4]1

参加物

4

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 4099083-Methoxycyclohexan-1-amine

生成物 1

HCID 86702165HCID 86702165、化合物収率 45%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a stirred solution of 3-methoxycyclohexanamine (0.200 g, 1.5 mmol) in pyridine (1 mL) was added methanesulfonyl chloride (0.144 mL, 1.9 mmol). The reaction mixture was stirred at room temperature for 16 hrs and then concentrated. The mixture was diluted with ethyl acetate and washed with 1 N aqueous hydrochloric acid, saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride, dried (anhydrous sodium sulfate), filtered, and concentrated to afford the product as a brown oil (0.140 g, 44%). The material was used without further purification.

後処理

  1. concentrationconcentrated
  2. additionThe mixture was diluted with ethyl acetate
  3. washwashed with 1 N aqueous hydrochloric acid, saturated aqueous sodium bicarbonate, saturated aqueous sodium chloride
  4. dry with materialdried (anhydrous sodium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-bcf2eab0cab446dca1017bad20bc964e
出典データセット
uspto-grants-2016_02
特許番号
US09265772B2

反応ノート

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