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Hydrochloric Acid → HCID 12958510、化合物

HRID 490476
ノート
印刷プレビュー

反応式

HRID 490476 の反応式
C([N:8]1[CH2:12][CH:11]2[C:13](=[O:23])[N:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:15](=[O:16])[CH:10]2[CH2:9]1)C1C=CC=CC=1.Cl.[OH-].[Na+]>C(O)C.[Pd]>[C:17]1([N:14]2[C:13](=[O:23])[CH:11]3[CH:10]([CH2:9][NH:8][CH2:12]3)[C:15]2=[O:16])[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 3564375-Benzyl-2-phenyltetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione

生成物 1

HCID 12958510HCID 12958510、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of 5-benzyl-2-phenyltetrahydropyrrolo[3,4-c]pyrrole-1,3-dione, freed of its hydrochloride beforehand by treatment with 4 N sodium hydroxide (93.2 g; 304 mmol), in absolute ethanol (1200 ml) is placed in a 5000 ml autoclave and palladium-on-charcoal at 5% (11 g) is then added. After having purged with nitrogen, the autoclave is placed under 64 bar of hydrogen at 70° C. for 12 hours. After returning to 20° C., the catalyst is filtered off and the filtrate is evaporated under reduced pressure. The compound obtained is triturated in diisopropyl ether (500 ml) and the solid obtained is filtered off, washed with diisopropyl ether and, finally, dried under reduced pressure at constant weight. 2-Phenyltetrahydropyrrolo[3,4-c]pyrrole-1,3-dione, (6.6 g; 92%) is isolated, the characteristics of which are as follows:

後処理

  1. additionis then added
  2. customAfter having purged with nitrogen
  3. customAfter returning to 20° C.
  4. filtrationthe catalyst is filtered off
  5. customthe filtrate is evaporated under reduced pressure
  6. customThe compound obtained
  7. customis triturated in diisopropyl ether (500 ml)
  8. customthe solid obtained
  9. filtrationis filtered off
  10. washwashed with diisopropyl ether
  11. customfinally, dried under reduced pressure at constant weight

出典と根拠

ORDレコード
ord-52c4c81f6fdb4d0aa79f269d36dccf3f
出典データセット
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07528147B2

反応ノート

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