Ammonium formate → HCID 54089766、化合物

HRID 429842ノート

反応式

HRID 429842 の反応式
Cl.[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][C@H:12]([N:14]([C@@H:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH3:19])[CH2:15][CH2:16][CH3:17])[CH3:13])=[CH:7][CH:6]=1)([O-])=O.C([O-])=O.[NH4+]>C(O)C.O.[Fe]>[NH2:2][C:5]1[CH:6]=[CH:7][C:8]([CH2:11][C@H:12]([N:14]([C@@H:18]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH3:19])[CH2:15][CH2:16][CH3:17])[CH3:13])=[CH:9][CH:10]=1

参加物

6

反応物 2

HCID 2723923Ammonium formateHCID 69143453HCID 69143453、化合物

生成物 1

HCID 54089766HCID 54089766、化合物

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

(R,R)-N-[2-(4-Nitrophenyl)-1-methylethyl]-N-propyl-(1-phenylethyl)amine hydrochloride was dissolved in ethanol (100 ml) and water (16 ml). To this solution was added iron powder (2.44 g) and ammonium formate (2.25 g). The mixture was heated at reflux for 3 hours, cooled to room temperature and filtered through a glass fiber filter. The filtrate was evaporated in vacuo, and the residue was partitioned between ethyl acetate and dilute sodium hydroxide. The organic layer was dried over sodium sulfate, filtered, and the solvent removed in vacuo to give (R,R)-N-[2-(4-aminophenyl)-1-methylethyl]-N-propyl-(1-phenylethyl)amine as a yellow syrup (2.9 g).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 3 hours
  3. filtrationfiltered through a glass fiber
  4. filtrationfilter
  5. customThe filtrate was evaporated in vacuo
  6. customthe residue was partitioned between ethyl acetate and dilute sodium hydroxide
  7. dry with materialThe organic layer was dried over sodium sulfate
  8. filtrationfiltered
  9. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-7fc6cc474dcd4f29a83c0a9f7d3dddad
出典データセット
uspto-grants-2001_11
特許番号
US06319920B1

反応ノート

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