Pyridine → HCID 12521647, compound

HRID 436139Notes

Reaction equation

HRID 436139 reaction equation
[CH2:1]([N:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][C:6](=[O:14])[C:5]2[CH2:15][S:16][CH2:17][C:4]1=2)[CH3:2].N1C=CC=CC=1.ClN1C(=O)CCC1=O>O>[CH2:1]([N:3]1[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[NH:7][C:6](=[O:14])[C:5]2=[CH:15][S:16][CH:17]=[C:4]12)[CH3:2]

Participants

5

Reactant 3

HCID 1049PyridineHCID 31398ChlorosuccinimideHCID 12521636HCID 12521636, compound

Product 1

HCID 12521647HCID 12521647, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a suspension of 0.246 g. of 4-ethyl-1,3,4,9-tetrahydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one in 2 ml. of dry pyridine is added in portions a total of 0.133 g. of N-chlorosuccinimide. The resulting solution is heated on a steam bath for 15 minutes, cooled and diluted with water. The solid is collected and recrystallized from methanol-water to give off-white crystals, m.p. 201°-202° C.

Workup

  1. additionTo a suspension of 0.246 g
  2. temperatureThe resulting solution is heated on a steam bath for 15 minutes
  3. temperaturecooled
  4. customThe solid is collected
  5. customrecrystallized from methanol-water
  6. customto give off-white crystals, m.p. 201°-202° C.

Sources & evidence

ORD record
ord-24fde611f7ad4d88b6c8c3428ef12c3b
Source dataset
uspto-grants-1977_02
Patent number
US04007272

Reaction notes

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