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

HRID 1638452ノート

反応式

HRID 1638452 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8d039b96c52c4204babea6ff1ea17f6c
出典データセット
uspto-grants-1989_11
特許番号
US04879391

反応ノート

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