Water → HCID 54046372、化合物

HRID 1074647ノート

反応式

HRID 1074647 の反応式
[C:1]([C:4]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH:5]=1)(=[O:3])[CH3:2].[CH3:16][Mg]Cl.O>O1CCCC1>[CH3:2][C:1]([CH3:16])([C:4]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH:5]=1)[OH:3]

参加物

5

反応物 3

HCID 962WaterHCID 1090051-(Cyclododec-1-en-1-yl)ethan-1-oneHCID 178418332HCID 178418332、化合物

生成物 1

HCID 54046372HCID 54046372、化合物収率 96%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

52 g (0.25 mole) of 1-acetyl-1-cyclododecene, prepared as described in Example 2, are added over 30 minutes to 200 ml of a 1.5-molar solution of methyl-magnesium chloride in tetrahydrofuran at from 0° to +10° C. After completion of the addition, the reaction mixture is hydrolyzed with 20 ml of water and the tetrahydrofuran solution is filtered to remove the salt which has precipitated. After destilling off the tetrahydrofuran under reduced pressure (50° C./20 mbars) the product which remains is fractionated. 52 g of dimethyl-cyclododecenyl-carbinol (96% yield) of boiling point=108°-112° C./0.01 mm Hg and refractive index nD25 =1.5000 are obtained.

後処理

  1. additionAfter completion of the addition
  2. filtrationthe tetrahydrofuran solution is filtered
  3. customto remove the salt which
  4. customhas precipitated
  5. customunder reduced pressure (50° C./20 mbars)

出典と根拠

ORDレコード
ord-755ca918e2e0460e9c573fe8196f2e3d
出典データセット
uspto-grants-1983_07
特許番号
US04393245

反応ノート

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