HCID 21451008, compound → HCID 86734519, compound

HRID 596199Notes

Reaction equation

HRID 596199 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[CH:17]=[C:16]([CH2:18][CH3:19])[S:15][C:10]=2[NH:11][CH2:12][CH2:13][N:14]=1.[N:20]1([CH2:26][CH2:27][NH:28][C:29]([Cl:31])=[O:30])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]1>N1C=CC=CC=1>[ClH:1].[ClH:31].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[CH:17]=[C:16]([CH2:18][CH3:19])[S:15][C:10]=2[N:11]([C:29](=[O:30])[NH:28][CH2:27][CH2:26][N:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)[CH2:12][CH2:13][N:14]=1

Participants

4

Reactant 2

HCID 21451008HCID 21451008, compoundHCID 135967971HCID 135967971, compound

Product 1

HCID 86734519HCID 86734519, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
60 °C

Procedure

To a solution of 5.8 g of 5-o-chlorophenyl-7-ethyl-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine in 50 ml of pyridine is added 4.2 g of 2-piperidinoethylcarbamoyl chloride, and the mixture is stirred for 24 hours at 60° C. Then pyridine is evaporated under reduced pressure, and to the residue is added acetone to crystallize. The crude crystals obtained are recrystallized from ethanol to give 5-o-chlorophenyl-7-ethyl-1-(2-piperidinoethylcarbamoyl)-2,3-dihydro-1H-thieno[2,3-e][1,4]diazepine dihydrochloride 1/2hydrate as yellow crystals, melting at 215°-216° C with decomposition.

Workup

  1. customThen pyridine is evaporated under reduced pressure
  2. additionto the residue is added acetone
  3. customto crystallize
  4. customThe crude crystals obtained
  5. customare recrystallized from ethanol

Sources & evidence

ORD record
ord-3e7c8e15e5ef4ea38cd07e833e3338be
Source dataset
uspto-grants-1977_03
Patent number
US04010184

Reaction notes

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