Hydrochloric Acid → HCID 21993733, compound

HRID 1978514Notes

Reaction equation

HRID 1978514 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:16][CH2:15][CH2:14][N:13]([C:17]([CH2:19][NH:20][C:21]([C:23]3[S:33][C:32]4[N:34]5[C:25](=[CH:26][N:27]=[C:28]5[CH:29]=[CH:30][CH:31]=4)[CH:24]=3)=[O:22])=[O:18])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:35]>C(O)C>[ClH:35].[ClH:35].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:16][CH2:15][CH2:14][N:13]([C:17]([CH2:19][NH:20][C:21]([C:23]3[S:33][C:32]4[N:34]5[C:25](=[CH:26][N:27]=[C:28]5[CH:29]=[CH:30][CH:31]=4)[CH:24]=3)=[O:22])=[O:18])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21993734HCID 21993734, compound

Product 1

HCID 21993733HCID 21993733, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.00 g (2.1 mmol.) of N-[4-(3-phenylpropan-1-yl)-2,3,5,6-tetrahydro-7H-1,4-diazepin-1-ylcarbonylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added, at room temperature, 1 ml (12 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes, followed by concentration under reduced pressure. To the resulting crystals was added diethyl ether. The crystals were collected by filtration, which were washed with ethanol and diethyl ether to give the object product as orange crystals. The yield was 0.996 g (86%).

Workup

  1. concentrationfollowed by concentration under reduced pressure
  2. additionTo the resulting crystals was added diethyl ether
  3. filtrationThe crystals were collected by filtration, which
  4. washwere washed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-672f393bfafc4a488ecf80d7e10afd13
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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