Hydrochloric Acid → HCID 20382079, compound

HRID 1448153Notes

Reaction equation

HRID 1448153 reaction equation
[Cl-:1].[Cl-].[Ca+2].[CH2:4]([N:6]1[C:14]2[N:13]=[C:12]3[CH:15](O)[C:16]4[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=4[CH2:18][CH2:19][C:11]3=[CH:10][C:9]=2[CH:8]=[N:7]1)[CH3:5].Cl>C1C=CC=CC=1>[Cl:1][CH:15]1[C:12]2=[N:13][C:14]3[N:6]([CH2:4][CH3:5])[N:7]=[CH:8][C:9]=3[CH:10]=[C:11]2[CH2:19][CH2:18][C:17]2[CH:20]=[CH:21][CH:22]=[CH:23][C:16]1=2

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 5284359Calcium ChlorideHCID 20382076HCID 20382076, compound

Product 1

HCID 20382079HCID 20382079, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

6 g. of pulverized CaCl2 are added with stirring to a solution of 11 g. of 1-ethyl-1,5,6,11-tetrahydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridin-11-ol (0.04 mol.), from example 2, in 175 ml. of dry benzene. The suspension is saturated for 15 hours with anhydrous hydrogen chloride at room temperature. After standing overnight, the mixture is filtered and the benzene is evaporated in vacuo. The residue is extracted with ether, treated with charcoal, and refrigerated to crystallize 8.3 g. of 11-chloro-1-ethyl-1,5,6,11-tetrahydrobenzo[5,6]cyclohepta[1,2-b]pyrazolo[4,3-e]pyridine; m.p. 107°-110° (ether).

Workup

  1. filtrationthe mixture is filtered
  2. customthe benzene is evaporated in vacuo
  3. extractionThe residue is extracted with ether
  4. additiontreated with charcoal
  5. customto crystallize 8.3 g

Sources & evidence

ORD record
ord-64461c5cec78452ea610ac644f59a58e
Source dataset
uspto-grants-1979_12
Patent number
US04179564

Reaction notes

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