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

HRID 1871913노트

반응식

HRID 1871913 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f3e389611c5448696ab82620b362106
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107307

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