Azobisisobutyronitrile → HCID 178459095、化合物

HRID 1972299

反応式

HRID 1972299 の反応式
CC(N=NC(C#N)(C)C)(C#N)C.C[CH2:14][C:15]([CH2:20][O:21][CH2:22][CH:23]=[CH2:24])(CO)CO.[C:25]([OH:30])(=[S:29])[CH:26]([CH3:28])[OH:27]>CO.C1(C)C=CC=CC=1.CCCCCC>[CH2:20]([O:21][CH2:22][CH:23]=[CH2:24])[CH:15]=[CH2:14].[C:25]([OH:30])(=[S:29])[CH:26]([CH3:28])[OH:27]

参加物

7

反応物 3

HCID 6547AzobisisobutyronitrileHCID 12683Trimethylolpropane monoallyl etherHCID 178473673HCID 178473673、化合物

生成物 1

HCID 178459095HCID 178459095、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 8058Hexane溶媒

反応条件

温度
90 °C

実験手順

AIBN (1.5 g) was dissolved in trimethylolpropane monoallyl ether (497 g, 2.86 mol). This solution was slowly added, under nitrogen with stirring, to thiolactic acid (300 g, 2.83 mol) at such a rate that the temperature of the exothermal reaction was kept at 80° C. When the addition was completed, the temperature was raised to 90° C. and kept at 90° C. for 1 h. The product had 1H-NMR (CDCl3): δ 1.11 (t, 3H, CH3CH2), 1.53 (q, 2H, CH3CH2), 2.00-2.20 (m, 2H, CH2CH2CH2), 2.98-3.06 (m, 2H, 3.65-4.02 (m, 9H); and is soluble in methanol and toluene, not soluble in hexane.

後処理

  1. additionThis solution was slowly added, under nitrogen
  2. customthat the temperature of the exothermal reaction
  3. customwas kept at 80° C
  4. additionWhen the addition

出典と根拠

ORDレコード
ord-641a1f01701d42dc9ace8d49418ea828
出典データセット
uspto-grants-2013_04
特許番号
US08431748B2

関連ノート

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