2,3-Dimethyl-1,3-butadiene → HCID 12477039、化合物

HRID 2050034ノート

反応式

HRID 2050034 の反応式
[CH2:1]([N:9]1[C:13](=[O:14])[CH:12]=[CH:11][S:10]1=[O:15])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8].[CH3:16][C:17]([C:19]([CH3:21])=[CH2:20])=[CH2:18]>C(Cl)CCl>[CH3:16][C:17]1[CH2:18][CH:12]2[C:13](=[O:14])[N:9]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH3:8])[S:10](=[O:15])[CH:11]2[CH2:20][C:19]=1[CH3:21]

参加物

4

反応物 2

HCID 105662,3-Dimethyl-1,3-butadieneHCID 159604752-Octyl-1H-1lambda~4~,2-thiazole-1,3(2H)-dione

生成物 1

HCID 12477039HCID 12477039、化合物収率 51%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
60 °C

実験手順

To a solution of 2.2 g (0.01 mole) of 2-n-octyl-4-isothiazolin-3-one 1-oxide in 15 ml of ethylene dichloride is added 1.1 g (0.012 mole) of 2,3-dimethyl-1,3-butadiene. The solution is stirred and maintained at 60° C. overnight. The mixture is concentrated to give a dark, thick oil. The oil is further purified by column chromatography (90% benzene, 10% acetone, silica) to yield 1.58 g (51%) of product as a yellow oil.

後処理

  1. concentrationThe mixture is concentrated
  2. customto give a dark, thick oil
  3. customThe oil is further purified by column chromatography (90% benzene, 10% acetone, silica)

出典と根拠

ORDレコード
ord-28404ea3b1684924a9bdac79e32e8ccb
出典データセット
uspto-grants-1980_04
特許番号
US04199591

反応ノート

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