1-Ethynylcyclohexanol → 1-Ethynylcyclohexyl methyl carbonate

HRID 258588

反応式

HRID 258588 の反応式
[C:1]([C:3]1([OH:9])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)#[CH:2].[Na].Cl[C:12]([O:14][CH3:15])=[O:13]>C1C=CC=CC=1.C1(C)C=CC=CC=1>[C:12](=[O:13])([O:9][C:3]1([C:1]#[CH:2])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)[O:14][CH3:15]

参加物

6

反応物 3

HCID 65251-EthynylcyclohexanolHCID 6586Methyl chloroformateHCID 5360545Sodium2 回

生成物 1

HCID 135708701-Ethynylcyclohexyl methyl carbonate

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 1140Toluene溶媒

実験手順

A solution of 36.0 gm of 1-ethynylcyclohexanol in 50 ml of benzene was slowly added drop-by-drop to an agitated suspension, cooled to 0° to 5° C., of 5.5 gm of finely distributed sodium in 50 ml of absolute toluene and 250 ml of benzene, and was agitated at room temperature until reaction had been completed. 26.0 gm of methyl chloroformate were added under cooling to the sodium salt which has been formed. The mixture was allowed to react for 12 hours at room temperature and was washed several times with water and dried. After distilling off the solvent, the raw ester was fractionated by means of a 20 cm Vigreux column. The methyl 1-ethynylcyclohexyl carbonate thus obtained constitutes a coloroless liquid having a fruity, herbal, complex odor and a distinctive fragrance of dill, and has the following characteristic values:

後処理

  1. customhas been formed
  2. customto react for 12 hours at room temperature
  3. washwas washed several times with water
  4. customdried
  5. distillationAfter distilling off the solvent

出典と根拠

ORDレコード
ord-2d4152fd3d184abaa38cef06fb156029
出典データセット
uspto-grants-1977_07
特許番号
US04033993

関連ノート

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