Water → 3-(Naphth-2-yl)-8-azabicyclo[3.2.1]octane oxalate

HRID 1871913ノート

反応式

HRID 1871913 の反応式
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11]1[CH2:17][CH:16]2[N:18](C([O:21][CH2:22][CH3:23])=O)[CH:13]([CH2:14][CH2:15]2)[CH2:12]1.[OH2:24].NN.[OH-:27].[K+].[OH2:29]>C(O)CO>[C:22]([OH:21])(=[O:29])[C:23]([OH:27])=[O:24].[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[CH:11]1[CH2:17][CH:16]2[NH:18][CH:13]([CH2:14][CH2:15]2)[CH2:12]1

参加物

6

反応物 4

HCID 962WaterHCID 14797Potassium HydroxideHCID 24654Hydrazine hydrate (1:1)HCID 186899083-(Naphth-2-yl)-8-ethoxycarbonyl-8-azabicyclo[3.2.1]octane

生成物 1

HCID 186899233-(Naphth-2-yl)-8-azabicyclo[3.2.1]octane oxalate

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

A mixture of 2.64 gm (8.53 mMol) 3-(naphth-2-yl)-8-ethoxycarbonyl-8-azabicyclo[3.2.1]octane, 2.14 gm (42.7 mMol) hydrazine hydrate, and 2.87 gm (51.2 mMol) potassium hydroxide in 70 mL ethylene glycol was heated at reflux for 2 hours. The reaction mixture was allowed to cool gradually to room temperature, poured into water and extracted well with diethyl ether. The organic phase was dried over sodium sulfate and concentrated under reduced pressure. The residue was treated with oxalic acid to provide the title compound.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. extractionextracted well with diethyl ether
  4. dry with materialThe organic phase was dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. additionThe residue was treated with oxalic acid

出典と根拠

ORDレコード
ord-5f3e389611c5448696ab82620b362106
出典データセット
uspto-grants-2000_08
特許番号
US06107307

反応ノート

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