Oxalic acid--4-(1-benzylpiperidin-3-yl)-1,2-phenylene diacetate (1/1) → Oxalic acid--4-(piperidin-3-yl)-1,2-phenylene diacetate (1/1)

HRID 2071417ノート

反応式

HRID 2071417 の反応式
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].C([N:14]1[CH2:19][CH2:18][CH2:17][CH:16]([C:20]2[CH:25]=[CH:24][C:23]([O:26][C:27](=[O:29])[CH3:28])=[C:22]([O:30][C:31](=[O:33])[CH3:32])[CH:21]=2)[CH2:15]1)C1C=CC=CC=1>C(O)C.[H][H]>[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[C:31]([O:30][C:22]1[CH:21]=[C:20]([CH:16]2[CH2:17][CH2:18][CH2:19][NH:14][CH2:15]2)[CH:25]=[CH:24][C:23]=1[O:26][C:27](=[O:29])[CH3:28])(=[O:33])[CH3:32]

参加物

4

反応物 1

HCID 3046215Oxalic acid--4-(1-benzylpiperidin-3-yl)-1,2-phenylene diacetate (1/1)

生成物 1

HCID 3046211Oxalic acid--4-(piperidin-3-yl)-1,2-phenylene diacetate (1/1)収率 40.5%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 178418361HCID 178418361、化合物溶媒2 回

実験手順

5 g of 10% palladized activated carbon were added to a solution of 10 g of the product of Step C in 600 ml of ethanol and hydrogen was introduced until hydrogen absorption ceased. The mixture was filtered and the filtrate was evaporated to dryness. The residue was dissolved in ethanol and the solution was cooled and vacuum filtered. The mother liquors were concentrated while progressively adding ethanol to a volume of 50 ml and was cooled and vacuum filtered. The recovered crystals were dried to obtain 3.25 g of 3-(3',4'-diacetoxyphenyl)-piperidine oxalate melting at 160° C.

後処理

  1. filtrationThe mixture was filtered
  2. customthe filtrate was evaporated to dryness
  3. dissolutionThe residue was dissolved in ethanol
  4. temperaturethe solution was cooled
  5. filtrationvacuum filtered
  6. concentrationThe mother liquors were concentrated while progressively adding ethanol to a volume of 50 ml
  7. temperaturewas cooled
  8. filtrationvacuum filtered
  9. customThe recovered crystals were dried

出典と根拠

ORDレコード
ord-b6de42f5ef29400aa1df73ae31ade5a8
出典データセット
uspto-grants-1977_09
特許番号
US04046901

反応ノート

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