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Fumaric Acid → HCID 70605269, 화합물

HRID 2163348
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HRID 2163348 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 444972Fumaric AcidHCID 54063020HCID 54063020, 화합물

생성물 1

HCID 70605269HCID 70605269, 화합물

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ddd4b9e51a70476daee927a76779d8f4
출처 데이터셋
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04133881

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