Pyridine → HCID 12521649, compound

HRID 436141Notes

Reaction equation

HRID 436141 reaction equation
[CH3:1][N:2]1[C:8]2[CH:9]=[C:10]([CH3:14])[C:11]([CH3:13])=[CH:12][C:7]=2[NH:6][C:5](=[O:15])[C:4]2[CH2:16][S:17][CH2:18][C:3]1=2.N1C=CC=CC=1.ClN1C(=O)CCC1=O>O>[CH3:1][N:2]1[C:8]2[CH:9]=[C:10]([CH3:14])[C:11]([CH3:13])=[CH:12][C:7]=2[NH:6][C:5](=[O:15])[C:4]2=[CH:16][S:17][CH:18]=[C:3]12

Participants

5

Reactant 3

HCID 1049PyridineHCID 31398ChlorosuccinimideHCID 12521638HCID 12521638, compound

Product 1

HCID 12521649HCID 12521649, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a suspension of 0.40 g. of 1,3,4,9-tetrahydro-4,6,7-trimethyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 3 ml. of dry pyridine is added, in portions, a total of 0.21 g. of N-chlorosuccinimide. The resulting solution is heated on a steam bath for 15 minutes, cooled and diluted with water. The solid which separates is collected and recrystallized from methanol to give yellow crystals, m.p. 260°-262° C.

Workup

  1. additionTo a suspension of 0.40 g
  2. temperatureThe resulting solution is heated on a steam bath for 15 minutes
  3. temperaturecooled
  4. customThe solid which separates is collected
  5. customrecrystallized from methanol
  6. customto give yellow crystals, m.p. 260°-262° C.

Sources & evidence

ORD record
ord-23bdcc88e4e241afb4f03a5681b817c9
Source dataset
uspto-grants-1977_02
Patent number
US04007272

Reaction notes

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