2,2-Dimethoxy-1-methylpyrrolidine → 1-(4-Methoxyphenyl)-3-(1-methyl-2-pyrrolidinylidene)-2(1H,3H)-indolone

HRID 1723540

반응식

HRID 1723540 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][C:10]2=[O:18])=[CH:5][CH:4]=1.CO[C:21]1(OC)[CH2:25][CH2:24][CH2:23][N:22]1[CH3:26]>C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11](=[C:21]3[CH2:25][CH2:24][CH2:23][N:22]3[CH3:26])[C:10]2=[O:18])=[CH:7][CH:8]=1

참가 물질

4

반응물 2

HCID 110735522,2-Dimethoxy-1-methylpyrrolidineHCID 133395441-(4-Methoxyphenyl)-1,3-dihydro-2H-indol-2-one

생성물 1

HCID 541264791-(4-Methoxyphenyl)-3-(1-methyl-2-pyrrolidinylidene)-2(1H,3H)-indolone

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

1-(4-Methoxyphenyl)-2(1H,3H)-indolone (49 g, 0.205 mole), N-methyl-2-pyrrolidone dimethyl acetal (ca. 80%, 53 g, 0.245 mole, Ber, 97, pp. 3081-7, 1964) and 1000 ml chloroform were refluxed under nitrogen for 1.5 hours. The reaction mixture was cooled and evaporated in vacuo to solids. Two recrystallizations from ethyl acetate gave purified title product, 44.7 g, m.p. 90°-93° C. Thirty grams of this material were dried at 80° C./15 mm Hg for 20 hours to give 26.1 g of title product, m.p. 127°-9° C.

후처리

  1. temperatureThe reaction mixture was cooled
  2. customevaporated in vacuo to solids
  3. customTwo recrystallizations from ethyl acetate
  4. customgave
  5. custompurified title product, 44.7 g, m.p. 90°-93° C
  6. dry with materialThirty grams of this material were dried at 80° C./15 mm Hg for 20 hours

출처 및 근거

ORD 기록
ord-b84c88baecb24707a4e1d7024a20efe7
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04861880

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