3-Methyl-2-buten-1-OL → 3-Methylbut-2-enyl 2-methylisocrotonate

HRID 65315

反応式

HRID 65315 の反応式
[C:1]([O:7][CH3:8])(=[O:6])/[C:2](=[CH:4]\[CH3:5])/[CH3:3].[CH3:9][C:10]([CH3:14])=[CH:11]CO.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCCCCCC)CCCCCCC.C([O-])(=O)CCCCCCCCCCC>C1(C)C=CC=CC=1>[C:1]([O:7][CH2:8][CH:9]=[C:10]([CH3:14])[CH3:11])(=[O:6])/[C:2](=[CH:4]\[CH3:5])/[CH3:3]

参加物

5

反応物 3

HCID 111733-Methyl-2-buten-1-OLHCID 5356352Methyl (2Z)-2-methyl-2-butenoateHCID 22292224Dioctyltin laurate

生成物 1

HCID 64329433-Methylbut-2-enyl 2-methylisocrotonate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 19.6 g. of methyl angelate, 22.2 g. of 3-methyl-2-butenyl alcohol, 100 ml. of toluene and 1.6 g. of dioctyltin laurate was placed in a glass flask which was equipped with a Soxhlet extractor filled with molecular sieve 4A on the top and a reflux cooler. The mixture was heated under reflux while returning the refluxed liquid through the molecular sieve 4A to the flask. The mixture obtained from the heating for a total of 26 hours was subjected to single distillation to give 24.24 g. of a distillate boiling at 102°-105° C. (25 mmHg).

後処理

  1. additionA mixture of 19.6 g
  2. customwhich was equipped with a Soxhlet extractor
  3. temperatureThe mixture was heated
  4. temperatureunder reflux
  5. customThe mixture obtained from the heating for a total of 26 hours
  6. distillationwas subjected to single distillation
  7. customto give 24.24 g

出典と根拠

ORDレコード
ord-08896e7ec06642c78abc4d95b1516e9c
出典データセット
uspto-grants-1986_09
特許番号
US04613680

関連ノート

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