Hydrochloric Acid → HCID 70296811, compound

HRID 1421212Notes

Reaction equation

HRID 1421212 reaction equation
[CH3:1][O:2][C:3]1[C:25]([O:26][CH3:27])=[CH:24][CH:23]=[CH:22][C:4]=1[CH:5]=[CH:6][C:7]1[C:13]2[CH:14]=[C:15]3[O:20][CH2:19][O:18][C:16]3=[CH:17][C:12]=2[CH2:11][C:10]([CH3:21])=[N:9][N:8]=1.[ClH:28]>C(OCC)(=O)C>[ClH:28].[CH3:1][O:2][C:3]1[C:25]([O:26][CH3:27])=[CH:24][CH:23]=[CH:22][C:4]=1[CH:5]=[CH:6][C:7]1[C:13]2[CH:14]=[C:15]3[O:20][CH2:19][O:18][C:16]3=[CH:17][C:12]=2[CH2:11][CH:10]([CH3:21])[NH:9][N:8]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54347453HCID 54347453, compound

Product 1

HCID 70296811HCID 70296811, compoundYield 45.8%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

1.5 g (4.12 mmoles) of 1-(2,3-dimethoxystyryl)-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine is reduced as specified in Example 1, the evaporation residue is dissolved in ethyl acetate and 10 ml of 10% by mass of ethyl acetate saturated with gaseous hydrogen chloride are added to the solution. The separated product is filtered, washed three times with 5 ml each of ethyl acetate and dried at a temperature between 80° C. and 100° C. Thus 0.76 g (45.8%) of the desired product is obtained. M.p.: 193-195° C. (decomp)

Workup

  1. filtrationThe separated product is filtered
  2. washwashed three times with 5 ml each of ethyl acetate
  3. customdried at a temperature between 80° C. and 100° C

Sources & evidence

ORD record
ord-91885e47faf6471b8124d9910d19bc9d
Source dataset
uspto-grants-2000_06
Patent number
US06075018

Reaction notes

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