Triethyl phosphonoacetate → HCID 86758349、化合物

HRID 2229244

反応式

HRID 2229244 の反応式
[C:1]([C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH3:14])[CH:10]=2)[CH:5]=1)(=O)[CH3:2].[H-].[Na+].C(OP([CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])(OCC)=O)C>C1COCC1>[CH3:14][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][CH:8]=1)[CH:5]=[C:4](/[C:1](/[CH3:2])=[CH:25]/[C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH:13]=[CH:12]2

参加物

5

反応物 3

HCID 13345Triethyl phosphonoacetateHCID 24758Sodium hydrideHCID 5980856'-Methyl-2'-acetonaphthone

生成物 1

HCID 86758349HCID 86758349、化合物収率 46.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-Acetyl-6-methylnaphthalene (5.08 g) was added to a cooled (0° C.) mixture of NaH (60% oil dispersion, 2.34 g) in THF (150 ml) and ethyl diethylphosphonoacetate (14.12 g) and the mixture was stirred at room temperature for 14 hours. The reaction was quenched by the addition of water. The organic layer was washed with water and brine, dried and concentrated. Recrystallization of the residue from hexane gave the titled compound (3.25 g) as a colorless solid.

後処理

  1. temperaturea cooled
  2. customThe reaction was quenched by the addition of water
  3. washThe organic layer was washed with water and brine
  4. customdried
  5. concentrationconcentrated
  6. customRecrystallization of the residue from hexane

出典と根拠

ORDレコード
ord-ea51eea4cc4c4c3995ef2fc70dde01a7
出典データセット
uspto-grants-2002_07
特許番号
US06420375B1

関連ノート

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