Oxalic Acid → HCID 11680498、化合物

HRID 2185671ノート

反応式

HRID 2185671 の反応式
[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]

参加物

5

反応物 2

HCID 971Oxalic AcidHCID 69969204HCID 69969204、化合物

生成物 1

HCID 11680498HCID 11680498、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6c6aea63739c4bd5b87b711aaff6c1fb
出典データセット
uspto-grants-2002_06
特許番号
US06403561B1

反応ノート

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