Amphetamine → HCID 70628179、化合物

HRID 616764ノート

反応式

HRID 616764 の反応式
C[CH:2](Cl)[C:3]([NH:5][C:6]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:7]=1[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:9])=[O:4].[CH3:22][CH:23]([NH2:31])[CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.O1CCOC[CH2:33]1>C(OCC)C>[ClH:20].[C:25]1([CH2:24][CH:23]([CH3:22])[NH:31][CH2:2][C:3]([N:5]([C:6]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:7]=2[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[O:9])[CH3:33])=[O:4])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 3007AmphetamineHCID 312751,4-DioxaneHCID 54271004HCID 54271004、化合物

生成物 1

HCID 70628179HCID 70628179、化合物収率 58%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

8 g of 2-(methyl-chloroacetamido)-5-chlorobenzophenone and 6.8 g of DL-amphetamine (= DL 1-phenyl-2-aminopropane) in 150 ml of anhydrous dioxan are heated to reflux for 4 hours whilst stirring. The turbid solution is filtered after cooling and evaporated in vacuo and the oily residue is triturated with three times 100 ml of water and dried in vacuo. The oily crude base (8.3 g) thus obtained is dissolved in 400 ml of anhydrous diethyl ether and filtered. 6.5 g of DL-2-(5-phenyl-N-methyl-4-methyl-3-aza-pentanamido)-5-chlorobenzophenone hydrochloride (58% of theory), with a melting point of 132°-135°, are obtained by passing in dry hydrogen chloride gas.

後処理

  1. temperatureto reflux for 4 hours
  2. filtrationThe turbid solution is filtered
  3. temperatureafter cooling
  4. customevaporated in vacuo
  5. customthe oily residue is triturated with three times 100 ml of water
  6. customdried in vacuo
  7. customThe oily crude base (8.3 g) thus obtained
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-d910216ed45646408a56561299c63c58
出典データセット
uspto-grants-1978_02
特許番号
US04075409

反応ノート

読み込み中…