Pyridine → alpha-Trifluoromethyl-3-phenoxybenzyl 3-(2,2-dimethylvinyl)-2,2-dimethylcyclopropanecarboxylate

HRID 261840

反応式

HRID 261840 の反応式
[CH3:1][C:2]1([CH3:12])[CH:4]([CH:5]=[C:6]([CH3:8])[CH3:7])[CH:3]1[C:9](Cl)=[O:10].[F:13][C:14]([F:31])([F:30])[CH:15]([OH:29])[C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([O:22][C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:17]=1.N1C=CC=CC=1>C1(C)C=CC=CC=1>[CH3:7][C:6]([CH3:8])=[CH:5][CH:4]1[CH:3]([C:9]([O:29][CH:15]([C:14]([F:13])([F:30])[F:31])[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:17]=2)=[O:10])[C:2]1([CH3:12])[CH3:1]

参加物

5

反応物 3

HCID 1049PyridineHCID 26620(1R-trans)-2,2-dimethyl-3-(2-methylprop-1-enyl)cyclopropanecarbonyl chlorideHCID 142705712,2,2-Trifluoro-1-(3-phenoxyphenyl)ethan-1-ol

生成物 1

HCID 12855315alpha-Trifluoromethyl-3-phenoxybenzyl 3-(2,2-dimethylvinyl)-2,2-dimethylcyclopropanecarboxylate収率 93.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

This compound was prepared in the manner of Example II using 3.3 g of 2,2-dimethyl-3-(2-methyl-1-propenyl)cyclopropanecarbonyl chloride, whose preparation is described in J. Sci. Food and Agriculture, 18, 325 (1967), 4.3 g of α-trifluoromethyl-3-phenoxybenzyl alcohol, and 1.5 g of pyridine in 50 ml of toluene. Volatiles were distilled from the crude reaction product at 90°/0.08 mm for 1/2 hour, then at 100°/0.08 mm for 3/4 hour through a short path Kugelrohr distillation system to give as a residue 6.3 g of α-trifluoromethyl-3-phenoxybenzyl 3-(2,2-dimethylvinyl)-2,2-dimethylcyclopropanecarboxylate. The ir spectrum was consistent with the assigned structure.

後処理

  1. customThis compound was prepared in the manner of Example II
  2. distillationVolatiles were distilled from the crude
  3. customreaction product at 90°/0.08 mm for 1/2 hour
  4. distillationat 100°/0.08 mm for 3/4 hour through a short path Kugelrohr distillation system

出典と根拠

ORDレコード
ord-50c25652e31947179f17951899bb060c
出典データセット
uspto-grants-1979_05
特許番号
US04152455

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