3-Nitroaniline → 3,3-Dimethyl-1-(3-nitrophenyl)pyrrolidine-2,5-dione

HRID 435043ノート

反応式

HRID 435043 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([CH:8]=[CH:9][CH:10]=1)[NH2:7])([O-:3])=[O:2].[CH3:11][C:12]([CH3:20])([CH2:16][C:17](O)=[O:18])[C:13](O)=[O:14]>C1(C)C(C)=CC=CC=1>[N+:1]([C:4]1[CH:5]=[C:6]([N:7]2[C:17](=[O:18])[CH2:16][C:12]([CH3:20])([CH3:11])[C:13]2=[O:14])[CH:8]=[CH:9][CH:10]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 74233-NitroanilineHCID 117012,2-Dimethylsuccinic acid

生成物 1

HCID 131892133,3-Dimethyl-1-(3-nitrophenyl)pyrrolidine-2,5-dione

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

Sixty-nine grams (0.5 mole) of m-nitroaniline and 76 grams (g.) (0.52 mole) of 2,2-dimethylsuccinic acid were mixed with 200 milliliters (ml.) of xylene and heated to reflux until approximately 20 ml. of water was removed in a modified Dean Stark apparatus. On cooling, the product crystallized from solution. The mixture was diluted with 300 ml. of ether, the solid filtered off, washed with an additional 100 ml. of ether and dried. Yield was 117.5 g. of a product having a melting point (m.p.) of 134°-134.5° C. The product was identified as the title compound by analysis of infrared spectra.

後処理

  1. temperatureheated
  2. temperatureto reflux until approximately 20 ml
  3. customof water was removed in a modified Dean Stark apparatus
  4. temperatureOn cooling
  5. customthe product crystallized from solution
  6. additionThe mixture was diluted with 300 ml
  7. filtrationof ether, the solid filtered off
  8. washwashed with an additional 100 ml
  9. dry with materialof ether and dried
  10. customa melting point (m.p.) of 134°-134.5° C

出典と根拠

ORDレコード
ord-8ba9e68e35b0463a81de96cfa51d8b02
出典データセット
uspto-grants-1983_08
特許番号
US04400202

反応ノート

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