1,5-Naphthalenedisulfonic acid → (3aRS,4SR,9aSR)-3a,4,9,9a-tetrahydro-4-phenyl-benz[f]isoindoline-2-propionic acid

HRID 426760

반응식

HRID 426760 반응식
C[O:2][C:3](=[O:25])[CH2:4][CH2:5][N:6]1[CH2:14][CH:13]2[CH:8]([CH:9]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH2:12]2)[CH2:7]1.[OH-].[Na+].C1(S(O)(=O)=O)C2C=CC=C(S(O)(=O)=O)C=2C=CC=1>Cl>[C:19]1([CH:9]2[CH:8]3[CH:13]([CH2:14][N:6]([CH2:5][CH2:4][C:3]([OH:25])=[O:2])[CH2:7]3)[CH2:12][C:11]3[CH:15]=[CH:16][CH:17]=[CH:18][C:10]2=3)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

참가 물질

5

반응물 3

HCID 66661,5-Naphthalenedisulfonic acidHCID 14798Sodium HydroxideHCID 70609075(3aRS,4SR,9aSR)-3a,4,9,9a-tetrahydro-4-phenyl-benz[f]isoindoline-2-propionic acid methyl ester

생성물 1

HCID 70610061(3aRS,4SR,9aSR)-3a,4,9,9a-tetrahydro-4-phenyl-benz[f]isoindoline-2-propionic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

10 g of (3aRS,4SR,9aSR)-3a,4,9,9a-tetrahydro-4-phenyl-benz[f]isoindoline-2-propionic acid methyl ester are heated to the boil at reflux in 50 cc of 2 N hydrochloric acid for 5 hours. The solution is then concentrated by evaporation, the residue is dissolved in water, the pH of the solution is adjusted to 1 with caustic soda solution, and 1 equivalent of 1,5-naphthalene disulphonic acid is added, whereby the bis-1,5-naphthalene-disulphonate salt form of the title compound is obtained in sticky form. The supernatant water is poured off and the resin is triturated with acetone, whereby it crystallizes. M.P. 193°-195°.

후처리

  1. concentrationThe solution is then concentrated by evaporation
  2. dissolutionthe residue is dissolved in water
  3. additionis added

출처 및 근거

ORD 기록
ord-5565e8652efa4e418f23c6459e25ff4c
출처 데이터셋
uspto-grants-1979_10
특허 번호
US04171369

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