Triethylamine → 2-Cyano-2-(2,4-dichlorophenyl)decyl methane sulfonate

HRID 616389ノート

反応式

HRID 616389 の反応式
[C:1]([C:3]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=1[Cl:21])([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH2:4][OH:5])#[N:2].[CH3:22][S:23](Cl)(=[O:25])=[O:24].C(N(CC)CC)C>C1C=CC=CC=1>[CH3:22][S:23]([O:5][CH2:4][C:3]([C:1]#[N:2])([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=1[Cl:21])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])(=[O:25])=[O:24]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 233398862-Cyano-2-(2,4-dichlorophenyl)decan-1-ol

生成物 1

HCID 233398942-Cyano-2-(2,4-dichlorophenyl)decyl methane sulfonate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a mixture of 2-cyano-2-(2,4-dichlorophenyl)decan-1-ol (40g., 0.12 mole) and methane sulfonyl chloride (15.3g., 0.13 mole) in 2 liters of benzene is added dropwise at 10° C., 14.8g., (0.14 mole) of triethylamine. The reaction mixture is stirred at room temperature for 30 minutes and then heated on a steam bath for another 30 minutes. The precipitate formed is filtered and the filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution and dried over magnesium sulfate. The solvent is evaporated to give 41.3g. of product, which is identified by nmr.

後処理

  1. additionis added dropwise at 10° C.
  2. temperatureheated on a steam bath for another 30 minutes
  3. customThe precipitate formed
  4. filtrationis filtered
  5. washthe filtrate is washed with dilute hydrochloric acid, water, saturated sodium bicarbonate solution, saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent is evaporated
  8. customto give 41.3g

出典と根拠

ORDレコード
ord-bd779e6425a449329db0520239f4d541
出典データセット
uspto-grants-1978_02
特許番号
US04073921

反応ノート

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