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Fumaric Acid → HCID 70605269、化合物

HRID 2163348
ノート
印刷プレビュー

反応式

HRID 2163348 の反応式
[C:1]1([C:7]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)([CH:11]2[CH2:14][N:13](C(C3C=CC=CC=3)C)[CH2:12]2)[C:8]([NH2:10])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]/[C:32]([OH:34])=[O:33]>[OH-].[OH-].[Pd+2].C(O)C>[C:29]([OH:36])(=[O:35])/[CH:30]=[CH:31]/[C:32]([OH:34])=[O:33].[C:1]1([C:7]([CH:11]2[CH2:14][NH:13][CH2:12]2)([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[C:8]([NH2:10])=[O:9])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 444972Fumaric AcidHCID 54063020HCID 54063020、化合物

生成物 1

HCID 70605269HCID 70605269、化合物

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

To a suspension of 23 g. (0.062 mole) of α,α-diphenyl-α-[1-(1-phenylethyl)-3-azetidinyl]acetamide in 150 ml. of ethanol solution was added 1.5 g. of 10% palladium hydroxide on carbon. The mixture was hydrogenated at 70° C. and an initial pressure of 45 p.s.i. for 18 hours and filtered. The filtrate was concentrated and the residue dissolved in 150 ml. of isopropyl alcohol. To this was added 7.2 g. (0.062 mole) of fumaric acid. The resulting crystals were recrystallized three times from ethanol to give 3 g. (13%) of product melting at 171°-173° C.

後処理

  1. additionTo a suspension of 23 g
  2. customwas hydrogenated at 70° C.
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated
  5. dissolutionthe residue dissolved in 150 ml
  6. additionTo this was added 7.2 g
  7. customThe resulting crystals were recrystallized three times from ethanol
  8. customto give 3 g

出典と根拠

ORDレコード
ord-ddd4b9e51a70476daee927a76779d8f4
出典データセット
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04133881

反応ノート

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