Acefylline → HCID 86734928, compound

HRID 258811Notes

Reaction equation

HRID 258811 reaction equation
[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([OH:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]>C(O)CC>[CH:1](=[C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10][NH2+:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1.[N:18]1([C:29](=[O:30])[C:28]2[N:27]([CH2:31][C:32]([O-:34])=[O:33])[CH:26]=[N:25][C:24]=2[N:22]([CH3:23])[C:20]1=[O:21])[CH3:19]

Participants

4

Reactant 2

HCID 69550AcefyllineHCID 70634238HCID 70634238, compound

Product 1

HCID 86734928HCID 86734928, compoundYield 48%

Reagents, catalysts & solvents 1

HCID 10311-PropanolSolvent

Procedure

2.21 g. (0.01 mole) of 1-benzal-1,2,3,4-tetrahydroisoquinoline and 2.38 g. (0.01 mole) of theophylline-7-acetic acid are dissolved under boiling in 25 ml. of n-propanol. The undissolved substances is filtered from the hot solution. The clear filtrate is crystallized while the mixture is cooled. The precipitated crystals are filtered out, covered with n-propanol and dried at room temperature. Thus 2.2 g. of 1-benzal-1,2,3,4-tetrahydroisoquinolinium-theophylline-7-acetate yield 48%) are obtained. Mp.: 168°-173° C. After recrystallization from a twofold amount of n-propanol the melting point was 195°-198° C.

Workup

  1. filtrationThe undissolved substances is filtered from the hot solution
  2. customThe clear filtrate is crystallized while the mixture
  3. temperatureis cooled
  4. filtrationThe precipitated crystals are filtered out
  5. customdried at room temperature

Sources & evidence

ORD record
ord-d139aa97146b4758aebd90d098d8954c
Source dataset
uspto-grants-1977_07
Patent number
US04035366

Reaction notes

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