Sodium Methoxide → 3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-dimethoxymethylpropanenitrile

HRID 34468

반응식

HRID 34468 반응식
[CH3:1][O-:2].[Na+].[CH3:4][O:5][C:6]1[CH:15]=[C:14]([CH:16]=[C:17]([CH2:20][O:21][CH3:22])[C:18]#[N:19])[C:9]2[CH:10]=[CH:11][CH2:12][O:13][C:8]=2[C:7]=1[O:23][CH3:24]>CO.O>[CH3:4][O:5][C:6]1[CH:15]=[C:14]([CH2:16][CH:17]([CH:20]([O:2][CH3:1])[O:21][CH3:22])[C:18]#[N:19])[C:9]2[CH:10]=[CH:11][CH2:12][O:13][C:8]=2[C:7]=1[O:23][CH3:24]

참가 물질

5

반응물 2

HCID 10942334Sodium MethoxideHCID 543734473-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile

생성물 1

HCID 201297603-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-dimethoxymethylpropanenitrile수율 62.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A mixture of sodium methoxide (8.86 g, 0.164 mole), and 3-(7,8-dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile (Example 37A, 23.1 g, 0.080 mole) in methanol (60 mL) was heated at reflux for 24 hr, allowed to cool and diluted with water (200 mL). The resultant mixture was extracted with toluene (1×200 mL and 2×100 mL). The combined toluene portions were extracted with water (3×100 mL) and dried over magnesium sulfate. The toluene solution was concentrated leaving a brown oil which was distilled under reduced pressure to give 15.9 g (62%) of a yellow oil which was used without further purification.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 24 hr
  3. temperatureto cool
  4. extractionThe resultant mixture was extracted with toluene (1×200 mL and 2×100 mL)
  5. extractionThe combined toluene portions were extracted with water (3×100 mL)
  6. dry with materialdried over magnesium sulfate
  7. concentrationThe toluene solution was concentrated
  8. customleaving a brown oil which
  9. distillationwas distilled under reduced pressure

출처 및 근거

ORD 기록
ord-00803f21b6de4e31b13e818b0ccc5ac9
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04761475

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