Hydrochloric Acid → HCID 19985919, compound

HRID 974341Notes

Reaction equation

HRID 974341 reaction equation
[ClH:1].[NH2:2][C:3]1[S:4][C:5]2[CH2:6][CH2:7][N:8]([CH2:13]/[CH:14]=[CH:15]/[C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[CH2:9][CH2:10][C:11]=2[N:12]=1>C(O)C>[ClH:1].[ClH:1].[NH2:2][C:3]1[S:4][C:5]2[CH2:6][CH2:7][N:8]([CH2:13]/[CH:14]=[CH:15]/[C:16]3[CH:17]=[CH:18][C:19]([C:22]#[N:23])=[CH:20][CH:21]=3)[CH2:9][CH2:10][C:11]=2[N:12]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 9819640HCID 9819640, compound

Product 1

HCID 19985919HCID 19985919, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

4.50 ml of 1N hydrochloric acid are added to 0.70 g (2.25 mmol) of (E)-2-amino-6-(3-(4-cyano-phenyl)allyl)-4,5,7,8-tetrahydro-6H-thiazolo[5,4-d]azepine in 10 ml of ethanol and heating is carried out until the solution is clear. Then it is evaporated to dryness in vacuo. ethanol is added to the foamy residue, it is evaporated down once more and this procedure with ethanol is repeated three times more. Then the product is dissolved in ethanol and heated ard cooled in ice. The crystals are filtered off and dried at 100° C./4 torr. Yield: 0.70 g (81% of theory), Melting point: 247°-250° C. (decomp.).

Workup

  1. temperatureheating
  2. customThen it is evaporated to dryness in vacuo
  3. additionethanol is added to the foamy residue, it
  4. customis evaporated down once more
  5. dissolutionThen the product is dissolved in ethanol
  6. temperatureheated ard
  7. temperaturecooled in ice
  8. filtrationThe crystals are filtered off
  9. customdried at 100° C./4 torr

Sources & evidence

ORD record
ord-f21152eee0cc4dc19c7cc456b48f5fca
Source dataset
uspto-grants-1991_11
Patent number
US05068325

Reaction notes

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