HCID 21584328、化合物 → HCID 21584267、化合物

HRID 583258ノート

反応式

HRID 583258 の反応式
[ClH:1].[N+:2]([C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH:10]3[N:15]([CH2:16][C:7]=2[CH:6]=1)[CH2:14][CH2:13][CH2:12][CH2:11]3)([O-])=O>C(O)C.[Pd]>[ClH:1].[CH2:11]1[CH:10]2[N:15]([CH2:16][C:7]3[CH:6]=[C:5]([NH2:2])[CH:18]=[CH:17][C:8]=3[CH2:9]2)[CH2:14][CH2:13][CH2:12]1

参加物

4

反応物 1

HCID 21584328HCID 21584328、化合物

生成物 1

HCID 21584267HCID 21584267、化合物収率 95.3%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

8-Nitro-1,3,4,6,11,11a-hexahydro-2H-benzo[b]quinolizine hydrochloride (2.93 g, 10.9 mmol) was dissolved in ethanol (150 ml) and 10% palladium-on-carbon (0.4 g) was added and the solution was shaken on a Parr Hydrogenator for 2 h. The catalyst was filtered off and the catalyst was washed with water. The filtrate was concentrated and absolute ethanol was added and evaporated to drive off excess water. The resulting solid was taken up in hot ethanol (75 ml) and ether (100 ml) was added slowly. The precipitate which formed was collected and dried in the air to give the title compound as an off-white solid (2.48 g, 95%), m.p. 241-3° C. (dec.).

後処理

  1. filtrationThe catalyst was filtered off
  2. washthe catalyst was washed with water
  3. concentrationThe filtrate was concentrated
  4. additionabsolute ethanol was added
  5. customevaporated
  6. additionether (100 ml) was added slowly
  7. customThe precipitate which formed
  8. customwas collected
  9. customdried in the air

出典と根拠

ORDレコード
ord-31dbfbf0d2d845288c6f33f8219b38a0
出典データセット
uspto-grants-1999_07
特許番号
US05929085

反応ノート

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