5-(Difluoromethyl)furan-2-carbaldehyde → 2-Furanmethanol, 5-(difluoromethyl)-alpha-ethynyl-

HRID 1654107ノート

反応式

HRID 1654107 の反応式
[C:1]([Mg]Br)#[CH:2].[F:5][CH:6]([F:14])[C:7]1[O:11][C:10]([CH:12]=[O:13])=[CH:9][CH:8]=1.P([O-])(O)(O)=O.[Na+]>O1CCCC1>[F:5][CH:6]([F:14])[C:7]1[O:11][C:10]([CH:12]([OH:13])[C:1]#[CH:2])=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 200796385-(Difluoromethyl)furan-2-carbaldehydeHCID 23672064Monosodium phosphateHCID 178418486HCID 178418486、化合物

生成物 1

HCID 200796722-Furanmethanol, 5-(difluoromethyl)-alpha-ethynyl-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

43 ml of a 0.5M solution of ethynyl magnesium bromide in tetrahydrofuran were added at 0° C. over one hour to a solution of 2.5 g of the product of Stage A and 30 ml of tetrahydrofuran. The reaction mixture was stirred at 0° C. for 1 hour and then was poured into a saturated aqueous sodium dihydrogenphosphate solution. The 3 g of product were chromatographed on silica by eluting with a 7/3 hexane/ethyl acetate mixture to obtain 2.5 g of the desired product.

後処理

  1. customThe 3 g of product were chromatographed on silica
  2. washby eluting with a 7/3 hexane/ethyl acetate mixture

出典と根拠

ORDレコード
ord-9687eb84b4484ce5bb90b631d8726245
出典データセット
uspto-grants-1995_04
特許番号
US05405865

反応ノート

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