HCID 12221967、化合物 → HCID 86754369、化合物

HRID 1584584ノート

反応式

HRID 1584584 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:14][C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7]1)=[O:5])[CH3:2].[H][H].C(OC(N1C[C@H]2[C@H](CCCC2)C1)=O)C>[C].[Rh].C(O)C>[CH2:1]([O:3][C:4]([N:6]1[CH2:7][C@H:8]2[C@@H:13]([CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:14]1)=[O:5])[CH3:2]

参加物

6

反応物 3

HCID 12221967HCID 12221967、化合物HCID 13097838Ethyl 1,3-dihydro-2H-isoindole-2-carboxylateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 86754369HCID 86754369、化合物収率 0.6%

試薬・触媒・溶媒 2

HCID 178503043HCID 178503043、化合物触媒HCID 702Ethanol溶媒

実験手順

In a 3-liter GL autoclave fitted with a electromagnetic stirrer are added 207 g of N-ethoxycarbonylisoindoline, 793 g of ethylalcohol and 20 g of 5% rhodium-carbon catalyst (50% water-containing). The reaction mixture is subjected to a hydrogen-pressure of 25 kg/cm2 and a temperature of 130° C. After a 10 hour hydrogen introduction, the drop in the rate of the hydrogen-absorption is observed, at this point the introduction of hydrogen is ceased to terminate the reaction. After the termination of reaction, the catalyst is filtered out from the reacted solution. By the result of the capillary chromatographic analysis, the yield of cis-hexahydro-N-ethoxycarbonylisoindoline is 95.3%. In addition, 0.6% of trans-hexahydro-N-ethoxycarbonylisoindoline is formed.

後処理

  1. customIn a 3-liter GL autoclave fitted with a electromagnetic stirrer
  2. customa temperature of 130° C
  3. customthe drop in the rate of the hydrogen-absorption
  4. customto terminate
  5. customthe reaction
  6. customAfter the termination of reaction
  7. filtrationthe catalyst is filtered out from the reacted solution
  8. customBy the result of the capillary chromatographic analysis

出典と根拠

ORDレコード
ord-034b8c9a734c4d5795201b41b3a1a7ad
出典データセット
uspto-grants-1999_08
特許番号
US05932744

反応ノート

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