Methane → HCID 178428206、化合物

HRID 268244

反応式

HRID 268244 の反応式
Cl.N([C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1)C1C=CC=CC=1.[Cl:23][C:24]1[CH:25]=[C:26]([CH:28]=[CH:29][C:30]=1[CH3:31])[NH2:27].C(O)C.C>CO>[ClH:23].[Cl:23][C:24]1[CH:25]=[C:26]([CH:28]=[CH:29][C:30]=1[CH3:31])[NH:27][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[C:16]3[N:21]=[CH:20][NH:19][C:17]3=2)[N:12]=[C:11]([CH3:22])[CH:10]=1

参加物

6

反応物 4

HCID 297MethaneHCID 702EthanolHCID 72553-Chloro-4-methylanilineHCID 178428198HCID 178428198、化合物

生成物 1

HCID 178428206HCID 178428206、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 500 ml., 3-neck, r.b. flask fitted with stirrer, condenser, and thermometer was charged with a mixture of the compound of Example I, C. (21.7 g., 0.1 mole), 3-chloro-4-methylaniline (14.2 g., 0.1 mole) and ethanol (300 ml.). The mixture was heated at reflux, while stirring, overnight. The near solution was concentrated to dryness by rotary evaporator and the residue was collected and dried to yield 35 g. (97.5%), m.p. 352°-364°C (dec). A 10 g. sample was dissolved in methanol (200 ml.), treated with charcoal and filtered while hot. Ether (ca 750 ml.) was added until the filtrate remained turbid and was then chilled. The crystals were collected by filtration and dried to yield 3.4 g. yellow crystals, m.p. 362°-370°C (dec). After two recrystallizations a m.p. 368°-372°C (dec) was obtained.

後処理

  1. customflask fitted with stirrer, condenser
  2. temperatureThe mixture was heated
  3. temperatureat reflux
  4. concentrationThe near solution was concentrated to dryness by rotary evaporator
  5. customthe residue was collected
  6. customdried
  7. customto yield 35 g
  8. filtrationfiltered while hot
  9. additionEther (ca 750 ml.) was added until the filtrate
  10. temperaturewas then chilled
  11. filtrationThe crystals were collected by filtration
  12. customdried
  13. customto yield 3.4 g
  14. customAfter two recrystallizations a m.p. 368°-372°C (dec)
  15. customwas obtained

出典と根拠

ORDレコード
ord-b80aeb6711fb4a458f42da2f0091e636
出典データセット
uspto-grants-1976_03
特許番号
US03947434

関連ノート

読み込み中…