Hydrochloric Acid → HCID 9819639, compound

HRID 974340Notes

Reaction equation

HRID 974340 reaction equation
[NH2:1][C:2]1[S:3][C:4]2[CH2:5][CH2:6][N:7]([CH2:12]/[CH:13]=[CH:14]/[C:15]3[CH:20]=[CH:19][C:18]([C:21]#[N:22])=[CH:17][CH:16]=3)[CH2:8][CH2:9][C:10]=2[N:11]=1.[ClH:23]>C(O)C>[ClH:23].[NH2:1][C:2]1[S:3][C:4]2[CH2:5][CH2:6][N:7]([CH2:12]/[CH:13]=[CH:14]/[C:15]3[CH:16]=[CH:17][C:18]([C:21]#[N:22])=[CH:19][CH:20]=3)[CH2:8][CH2:9][C:10]=2[N:11]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 9819640HCID 9819640, compound

Product 1

HCID 9819639HCID 9819639, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2.25 ml of IN 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 the mixture is heated until the solution is clear. It is then cooled in an ice bath. The slowly precipitated crystals are filtered off. After washing with ethanol and with ether and drying at 100° C./4 torr, the monohydrochloride is obtained. Yield: 0.46 g (59% of theory), Melting point: 237° C. (decomp.).

Workup

  1. temperaturethe mixture is heated until the solution
  2. temperatureIt is then cooled in an ice bath
  3. filtrationThe slowly precipitated crystals are filtered off
  4. washAfter washing with ethanol and with ether
  5. customdrying at 100° C./4 torr

Sources & evidence

ORD record
ord-e2720f4c2bbc4e37b2abbcddf6ebd06b
Source dataset
uspto-grants-1991_11
Patent number
US05068325

Reaction notes

Loading…