2,3-Dimethylcyclohexan-1-ol → sec-Butyl-carbamic acid 2,3-dimethyl-cyclohexyl ester

HRID 1472238ノート

反応式

HRID 1472238 の反応式
[CH:1]([N:5]=[C:6]=[O:7])([CH2:3][CH3:4])[CH3:2].[CH3:8][CH:9]1[CH:14]([CH3:15])[CH2:13][CH2:12][CH2:11][CH:10]1[OH:16]>O>[CH3:8][CH:9]1[CH:14]([CH3:15])[CH2:13][CH2:12][CH2:11][CH:10]1[O:16][C:6](=[O:7])[NH:5][CH:1]([CH2:3][CH3:4])[CH3:2]

参加物

4

反応物 2

HCID 1026312,3-Dimethylcyclohexan-1-olHCID 5508502-Isocyanatobutane

生成物 1

HCID 46898981sec-Butyl-carbamic acid 2,3-dimethyl-cyclohexyl ester収率 53%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

50.7 g (0.5 mol) sec.-Butyl isocyanate were placed in a 500 ml vessel at ambient temperature and 64.1 g (0.5 mol) 2,3-dimethylcyclohexanol were added. The reaction mixture was heated for 5 h to 150° C., cooled and subsequently 100 ml water were added. After refluxing for one hour the solution was cooled down, the phases separated and extracted once with MTBE (methyl tert.-butyl ether). The raw product was purified by distillation to yield 60.2 g product as a mixture of isomers with a purity of 99.6%.

後処理

  1. temperatureThe reaction mixture was heated for 5 h to 150° C.
  2. temperaturecooled
  3. temperatureAfter refluxing for one hour the solution
  4. temperaturewas cooled down
  5. customthe phases separated
  6. extractionextracted once with MTBE (methyl tert.-butyl ether)
  7. distillationThe raw product was purified by distillation

出典と根拠

ORDレコード
ord-2ae43b0fdef44f85b70cfd7229cce8df
出典データセット
uspto-grants-2015_04
特許番号
US09012497B2

反応ノート

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