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Sodium → HCID 23316502, compound

HRID 1982455
Notes
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Reaction equation

HRID 1982455 reaction equation
[Na].[CH2:2]([O:4][C:5]([C:7]1[N:8]=[CH:9][C:10]2[NH:11][C:12]3[C:17]([C:18]=2[C:19]=1[CH2:20][O:21][CH3:22])=[CH:16][CH:15]=[CH:14][CH:13]=3)=[O:6])C.P([O-])(O)(O)=O.[Na+]>CO>[CH3:2][O:4][C:5]([C:7]1[N:8]=[CH:9][C:10]2[NH:11][C:12]3[C:17]([C:18]=2[C:19]=1[CH2:20][O:21][CH3:22])=[CH:16][CH:15]=[CH:14][CH:13]=3)=[O:6]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 5360545SodiumHCID 13041786HCID 13041786, compoundHCID 23672064Monosodium phosphate

Product 1

HCID 23316502HCID 23316502, compoundYield 94.7%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

30 mg of sodium is dissolved in 15 ml of absolute methanol. Then, 300 mg of 4-methoxymethyl-beta-carboline-3-carboxylic-acid-ethylester is added and the mixture is heated with reflux for 2 h. The cooled solution is poured into a sodium dihydrogen phosphate solution and extracted with ethyl acetate. Crystallization in hexane/methylene-chloride yields 270 mg of 4-methoxymethyl-beta-carboline-3-carboxylic-acid-methylester with a m.p. 134°-135° C.

Workup

  1. temperaturethe mixture is heated
  2. temperaturewith reflux for 2 h
  3. extractionextracted with ethyl acetate
  4. customCrystallization in hexane/methylene-chloride

Sources & evidence

ORD record
ord-2abef2d825b64ae6bfdefe2064c04cfd
Source dataset
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04596808

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes