Hydrochloric Acid → HCID 86753946, compound

HRID 1418921Notes

Reaction equation

HRID 1418921 reaction equation
[CH2:1]([N:4]([CH2:8][C:9]1[O:13][C:12]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][S:26][C:22]=4[C:21](=[O:27])[N:20]([CH3:28])[CH2:19][C:18]=23)=[N:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3].[ClH:29]>C(OCC)(=O)C>[ClH:29].[CH2:1]([N:4]([CH2:8][C:9]1[O:13][C:12]([C:14]2[N:15]=[CH:16][N:17]3[C:23]4[CH:24]=[CH:25][S:26][C:22]=4[C:21](=[O:27])[N:20]([CH3:28])[CH2:19][C:18]=23)=[N:11][CH:10]=1)[CH2:5][CH2:6][CH3:7])[CH2:2][CH3:3]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21842240HCID 21842240, compound

Product 1

HCID 86753946HCID 86753946, compoundYield 85.1%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

1.13 g (0.00283 mol) of 3-(5-dipropylaminomethyl-oxazol-2-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a]thieno[2,3-f][1,4]-diazepin-6-one in 50 ml of ethyl acetate were treated with 0.84 ml (0.00311 mol) of 3.7N ethanolic hydrochloric acid. After stirring at 0° for 1/2 hr. the suspension was suction filtered. The yellowish crystals were dissolved in hot acetonitrile and recrystallized by the addition of ether. There were obtained 1.05 g (85%) of 3-(5-dipropylaminomethyl-oxazol-2-yl)-5-methyl-5,6-dihydro-4H-imidazo[1,5-a]thieno[2,3-f][1,4]diazepin-6-one hydrochloride (1:1) as light beige crystals; m.p. 237°-241° (dec.).

Workup

  1. filtrationsuction filtered
  2. dissolutionThe yellowish crystals were dissolved in hot acetonitrile
  3. customrecrystallized by the addition of ether

Sources & evidence

ORD record
ord-1fc75538f5b944fcb41a1c5aed0aaf40
Source dataset
uspto-grants-1999_03
Patent number
US05885986

Reaction notes

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