HCID 12680127, compound → HCID 12680131, compound

HRID 1855731Notes

Reaction equation

HRID 1855731 reaction equation
[NH2:1][C:2]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:3]=1[C:4]([NH:6][C:7]1[C:11](OCC)=[CH:10][S:9][CH:8]=1)=[O:5]>O>[F:19][C:16]1[CH:17]=[CH:18][C:2]2[NH:1][C:11]3=[CH:10][S:9][CH:8]=[C:7]3[NH:6][C:4](=[O:5])[C:3]=2[CH:15]=1

Participants

3

Reactant 1

HCID 12680127HCID 12680127, compound

Product 1

HCID 12680131HCID 12680131, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A 5.7 g. portion of 2-amino-N-(4-ethoxy-3-thienyl)-5-fluorobenzamide and 60 g. of polyphosphoric acid are stirred and heated at 120°-128° C. for one hour, cooled and poured into ice and water. The solid is recovered by filtration, washed with water, sodium carbonate solution, sodium bicarbonate solution and then water and dried at 60° C. overnight, giving 7-fluoro-4H-thieno[3,4-b][1,4]benzodiazepin-9(10H)-one.

Workup

  1. temperatureheated at 120°-128° C. for one hour
  2. temperaturecooled
  3. filtrationThe solid is recovered by filtration
  4. washwashed with water, sodium carbonate solution, sodium bicarbonate solution
  5. dry with materialwater and dried at 60° C. overnight

Sources & evidence

ORD record
ord-1cb0124583994f678c883587f834d1fd
Source dataset
uspto-grants-1980_08
Patent number
US04216148

Reaction notes

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