Methylamine → HCID 13457740、化合物

HRID 280121ノート

反応式

HRID 280121 の反応式
[Cl:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[C:4]([C:6]1[N:7]([N:11]2C(=O)C3=CC=CC=C3C2=O)[CH:8]=[CH:9][CH:10]=1)=[O:5].CN>C(O)C.O>[NH2:11][N:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4](=[O:5])[C:3]1[CH:22]=[CH:23][CH:24]=[CH:25][C:2]=1[Cl:1]

参加物

5

実験手順

2-(2-chlorobenzoyl)-1-phthalimidopyrrole (40 g, 0.114 mol) was suspended in 350 ml of 95% ethanol. To this rapidly stirred slurry was added 50 ml of a 40% aqueous solution of methylamine over 10 minutes. After 2.5 hours of rapid stirring the mixture was diluted with 400 ml of water and extracted with four 200 ml portions of ether. The combined extracts were washed with water, dried over anhydrous MgSO4, filtered and evaporated to an oil which solidified upon standing. Trituration of this solid with hexane and collection upon a filter yielded 23.6 g (94%) of solid, m.p. 76°-78°.

後処理

  1. extractionextracted with four 200 ml portions of ether
  2. washThe combined extracts were washed with water
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. customevaporated to an oil which
  6. customTrituration of this solid with hexane and collection upon a filter

出典と根拠

ORDレコード
ord-8e022944b64b4969b119949d3c48572c
出典データセット
uspto-grants-1986_05
特許番号
US04588727

反応ノート

読み込み中…