Sulfuric Acid → 1-[(2,2,6-Trimethylcyclohexyl)oxy]pentan-2-OL

HRID 365172

反応式

HRID 365172 の反応式
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[OH:10].[H-].[Na+].[O:13]1[CH:15]([CH2:16][CH2:17][CH3:18])[CH2:14]1.OS(O)(=O)=O>C1(C)C=CC=CC=1>[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[CH:3]1[O:10][CH2:14][CH:15]([OH:13])[CH2:16][CH2:17][CH3:18]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 13853Oxirane, 2-propyl-HCID 24758Sodium hydrideHCID 125371292,2,6-Trimethylcyclohexan-1-ol

生成物 1

HCID 30211651-[(2,2,6-Trimethylcyclohexyl)oxy]pentan-2-OL収率 75%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2.0 g of 2,6,6-trimethyl-cyclohexanol and 0.354 g of sodium hydride was heated for 24 hours at 80° in 10 ml of anhydrous toluene. 1.2 G of 1,2-epoxy-pentane were then added to the thus obtained solution and heating at 80° was maintained for 24 additional hours. After cooling, the reaction mixture was poured onto crushed iced, acidified with diluted H2SO4, whereupon the organic phase was washed with brine until neutrality. After evaporation of the volatile parts and distillation of the residue in a a bulb apparatus (bath temperature: 140°/7 Pa), the desired product was obtained in yield of about 75%. An analytical sample was purified by preparative gas chromatography.

後処理

  1. temperatureheating at 80°
  2. temperaturewas maintained for 24 additional hours
  3. temperatureAfter cooling
  4. additionthe reaction mixture was poured
  5. customonto crushed iced
  6. washwas washed with brine until neutrality
  7. customAfter evaporation of the volatile parts and distillation of the residue in a a bulb apparatus (bath temperature: 140°/7 Pa)

出典と根拠

ORDレコード
ord-f4e9b88607ef45dab5742f8501ec720f
出典データセット
uspto-grants-1986_08
特許番号
US04608445

関連ノート

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