2'-Hydroxy-4',6'-bis(methoxymethoxy)-3'-(3-methyl2-butenyl)acetophenone → 2'-Hydroxy-3'-isopentyl-4',6'-bis(methoxymethoxy)acetophenone

HRID 1030690

反応式

HRID 1030690 の反応式
[OH:1][C:2]1[C:7]([CH2:8][CH:9]=[C:10]([CH3:12])[CH3:11])=[C:6]([O:13][CH2:14][O:15][CH3:16])[CH:5]=[C:4]([O:17][CH2:18][O:19][CH3:20])[C:3]=1[C:21](=[O:23])[CH3:22].[H][H]>C(O)C>[OH:1][C:2]1[C:7]([CH2:8][CH2:9][CH:10]([CH3:12])[CH3:11])=[C:6]([O:13][CH2:14][O:15][CH3:16])[CH:5]=[C:4]([O:17][CH2:18][O:19][CH3:20])[C:3]=1[C:21](=[O:23])[CH3:22]

参加物

4

反応物 2

HCID 110993722'-Hydroxy-4',6'-bis(methoxymethoxy)-3'-(3-methyl2-butenyl)acetophenoneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 160945312'-Hydroxy-3'-isopentyl-4',6'-bis(methoxymethoxy)acetophenone収率 82.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2.08 g of the 2'-hydroxy-4',6'-bis(methoxymethoxy)-3'-(3-methyl-2-butenyl)acetophenone obtained in Production Example 13 in ethanol (20 ml) was added to a sufficiently hydrogen gas-absorbed suspension of 1.0 g of 5% palladium-carbon in 30 ml of ethanol, and the mixture was stirred at room temperature under atmospheric pressure in a hydrogen atmosphere. After the reaction, the reaction mixture was filtered, and the solvent was removed from the filtrate by distillation. The obtained residue was subjected to the silica gel column chromatography (3.0 cm in diameter, 60 g of silica gel, 0.3 kg/cm2) using a mixed solvent of n-hexane and ethyl acetate (n-hexane/ethyl acetate-3/1). Fractions of 50 ml were recovered, and 1.73 g (yield=82.8%) of 2'-hydroxy-3'-isopentyl-4',6'-bis(methoxymethoxy)acetophenone in the form of a yellow oil was obtained from the third to fifth fractions.

後処理

  1. customgas-absorbed
  2. additionsuspension of 1.0 g of 5% palladium-carbon in 30 ml of ethanol
  3. customAfter the reaction
  4. filtrationthe reaction mixture was filtered
  5. customthe solvent was removed from the filtrate by distillation
  6. customFractions of 50 ml were recovered

出典と根拠

ORDレコード
ord-947296a762f14e6da0e7590ae1fa0b2e
出典データセット
uspto-grants-1992_04
特許番号
US05106871

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