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 2071417노트

반응식

HRID 2071417 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 178418361HCID 178418361, 화합물용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b6de42f5ef29400aa1df73ae31ade5a8
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046901

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