Sulfuric Acid → 3-(4,4-Dimethyl-cyclohex-1-enyl)-propionic acid butyl ester

HRID 585465

反応式

HRID 585465 の反応式
[CH3:1][C:2]1([CH3:13])[CH2:12][CH2:11][C:5]2([O:9][C:8](=[O:10])[CH2:7][CH2:6]2)[CH2:4][CH2:3]1.OS(O)(=O)=O>C(O)CCC>[CH2:1]([O:9][C:8](=[O:10])[CH2:7][CH2:6][C:5]1[CH2:11][CH2:12][C:2]([CH3:13])([CH3:1])[CH2:3][CH:4]=1)[CH2:2][CH2:3][CH3:4]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 134091248,8-Dimethyl-1-oxa-spiro[4.5]decan-2-one

生成物 1

HCID 236558383-(4,4-Dimethyl-cyclohex-1-enyl)-propionic acid butyl ester

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒2 回

実験手順

The crude 8,8-dimethyl-1-oxa-spiro[4.5]decan-2-one (40.2 g, 0.22 mol) was introduced into a 250 ml three necked round bottom flask together with butanol (23 g) and concentrated H2SO4 (0.5 g). Temperature was risen to 140° C. and during 8 hours fresh butanol (42.9 g) was introduced, while collecting a mixture of butanol/water. The reaction mixture was cooled to room temperature and toluene (66 g) and water (66 g) were added. The organic phase was washed with NaHCO3 and water to yield after concentration 51.42 g of the desired compound. Flash distillation (68°–70° C., 0.2 hPa) led to 35.0 g of butylester (overall yield: 47%; GC purity: 96.0%).

後処理

  1. customwhile collecting
  2. additiona mixture of butanol/water
  3. additiontoluene (66 g) and water (66 g) were added
  4. washThe organic phase was washed with NaHCO3 and water

出典と根拠

ORDレコード
ord-0d16dd0ef4a845798ff4baff7b4ef04d
出典データセット
uspto-grants-2005_08
特許番号
US06933265B2

関連ノート

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