Triethyl phosphonoacetate → HCID 86758349, 화합물

HRID 2229244

반응식

HRID 2229244 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 86758349HCID 86758349, 화합물수율 46.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ea51eea4cc4c4c3995ef2fc70dde01a7
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420375B1

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