Oxalic Acid → HCID 11680498, 화합물

HRID 2185671노트

반응식

HRID 2185671 반응식
[CH3:1][NH:2][C:3]([C@@H:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]1[C:14](=[O:29])[C@@H:15]([NH:18]C(OCC1C=CC=CC=1)=O)[CH2:16][CH3:17])=[O:4].C(O)(=O)C(O)=O>CO.[Pd]>[CH3:1][NH:2][C:3]([C@@H:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[N:6]1[C:14](=[O:29])[C@@H:15]([NH2:18])[CH2:16][CH3:17])=[O:4]

참가 물질

5

반응물 2

HCID 971Oxalic AcidHCID 69969204HCID 69969204, 화합물

생성물 1

HCID 11680498HCID 11680498, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

2.15 g (5.44 mmol) of the compound obtained in step d) are dissolved in 200 ml of methanol and 0.85 g of activated 10% palladium-on-charcoal (wet) is added. The reaction mixture is hydrogenated at 60 psi for 3 hours. The solution is filtered and 1.3 equivalents (0.64 g) of oxalic acid (7.07 mmol) are added and the solution is then concentrated under vacuum. Ethanol is added, followed by ether (1:50 ratio) and a crystallized product is obtained. After filtration and washing with diethyl ether, the solid is dried under vacuum for 24 hours over P2O5 at 35° C. The desired product is obtained.

후처리

  1. filtrationThe solution is filtered
  2. concentrationthe solution is then concentrated under vacuum
  3. additionEthanol is added
  4. customa crystallized product is obtained
  5. filtrationAfter filtration
  6. washwashing with diethyl ether
  7. dry with materialthe solid is dried under vacuum for 24 hours over P2O5 at 35° C

출처 및 근거

ORD 기록
ord-6c6aea63739c4bd5b87b711aaff6c1fb
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06403561B1

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