HCID 70296521, compound → HCID 54028746, compound

HRID 1421215Notes

Reaction equation

HRID 1421215 reaction equation
[NH2:1][C:2]1[CH:25]=[CH:24][C:5]([CH:6]=[CH:7][C:8]2[C:14]3[CH:15]=[C:16]([O:21][CH3:22])[C:17]([O:19][CH3:20])=[CH:18][C:13]=3[CH2:12][CH:11]([CH3:23])[NH:10][N:9]=2)=[CH:4][CH:3]=1>C(OC(=O)C)(=O)C>[C:17]([NH:1][C:2]1[CH:25]=[CH:24][C:5]([CH:6]=[CH:7][C:8]2[C:14]3[CH:15]=[C:16]([O:21][CH3:22])[C:17]([O:19][CH3:20])=[CH:18][C:13]=3[CH2:12][CH:11]([CH3:23])[N:10]([C:16](=[O:21])[CH3:15])[N:9]=2)=[CH:4][CH:3]=1)(=[O:19])[CH3:18]

Participants

3

Reactant 1

HCID 70296521HCID 70296521, compound

Product 1

HCID 54028746HCID 54028746, compoundYield 142.8%

Reagents, catalysts & solvents 1

HCID 7918Acetic AnhydrideSolvent

Procedure

1.2 g (3.56,mmoles) of 1-(4-aminostyryl)-4-methyl-7,8-dimethoxy-3,4-dihydro-5H-2,3-benzodiazepine prepared according to Example 33 is suspended in 6 ml of acetic anhydride. The suspension is stirred for 1 hour at room temperature. In the meantime the starting compound gets dissolved, the end-product begins to separate and the reaction mixture gets thick. The separated product is filtered off, washed three times with 15 ml each of diethyl ether and dried at a temperature between 80° C. and 100° C. Thus 1.07 g (71.3%) of the desired compound is obtained.

Workup

  1. dissolutionIn the meantime the starting compound gets dissolved
  2. customto separate
  3. filtrationThe separated product is filtered off
  4. washwashed three times with 15 ml each of diethyl ether
  5. customdried at a temperature between 80° C. and 100° C

Sources & evidence

ORD record
ord-f4174ff51da241c1813447c69df03813
Source dataset
uspto-grants-2000_06
Patent number
US06075018

Reaction notes

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