Hydrochloric Acid → HCID 9845976, compound

HRID 2298049Notes

Reaction equation

HRID 2298049 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([NH:14]C(=O)OC(C)(C)C)[CH2:10][CH2:9]2)=[CH:4][C:3]=1[C:22]([NH:24][CH2:25][C:26]12[CH2:35][CH:30]3[CH2:31][CH:32]([CH2:34][CH:28]([CH2:29]3)[CH2:27]1)[CH2:33]2)=[O:23].Cl.CO>O1CCOCC1>[ClH:1].[NH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[C:3]([CH:4]=2)[C:22]([NH:24][CH2:25][C:26]23[CH2:35][CH:30]4[CH2:31][CH:32]([CH2:34][CH:28]([CH2:29]4)[CH2:27]2)[CH2:33]3)=[O:23])[CH2:9][CH2:10]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 57244288HCID 57244288, compound

Product 1

HCID 9845976HCID 9845976, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Prepared as described in example 5d) above using [1-[4-chloro-3-[[(tricyclo[3.3.1.13,7]dec-1-ylmethyl)amino]carbonyl]phenyl]-4-piperidinyl]-carbamic acid, 1,1-dimethylethyl ester (Example 6c), hydrochloric acid (0.5 ml of a 4N solution in dioxane) and methanol (10 ml). The mixture was heated at reflux for 15 min. to complete the reaction. After evaporation to two-thirds of the original volume, a solid crystallised on standing which was collected by filtration and dried in vacuo to give the title compound as a solid (0.025 g).

Workup

  1. customPrepared
  2. temperatureThe mixture was heated
  3. temperatureat reflux for 15 min.
  4. customthe reaction
  5. customAfter evaporation to two-thirds of the original volume
  6. customa solid crystallised on standing which
  7. filtrationwas collected by filtration
  8. customdried in vacuo

Sources & evidence

ORD record
ord-55b630f7cee045b3b66bd808466296d6
Source dataset
uspto-grants-2002_12
Patent number
US06492355B1

Reaction notes

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