Hydrochloric Acid → HCID 131723702, compound

HRID 2298103Notes

Reaction equation

HRID 2298103 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)=[CH:4][C:3]=1[C:22]([NH:24][CH2:25][CH2:26][C:27]12[CH2:36][CH:31]3[CH2:32][CH:33]([CH2:35][CH:29]([CH2:30]3)[CH2:28]1)[CH2:34]2)=[O:23].Cl>CO.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][C:3]=1[C:22]([NH:24][CH2:25][CH2:26][C:27]12[CH2:34][CH:33]3[CH2:35][CH:29]([CH2:30][CH:31]([CH2:32]3)[CH2:36]1)[CH2:28]2)=[O:23]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 57022441HCID 57022441, compound

Product 1

HCID 131723702HCID 131723702, compoundYield 73.2%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent

Procedure

4-[4-Chloro-3-[[(2-tricyclo[3.3.1.13,7]dec-1-ylethyl)amino]carbonyl]phenyl]-hexahydro-1H-1,4-diazepine-1-carboxylic acid, 1,1-dimethylethyl ester (0.053 g, Example 74a) was dissolved in methanol (5 ml) and hydrochloric acid (0.5 ml from a 4N solution in dioxane) was added. After stirring at room temperature for 14 h, the mixture was evaporated to ¾ original volume under reduced pressure. Diethyl ether was gradually added to the solution and the resulting precipitate was collected by filtration, washed with diethyl ether and dried in vacuo to afford the title compound as a cream solid (0.017 g).

Workup

  1. customthe mixture was evaporated
  2. additionDiethyl ether was gradually added to the solution
  3. filtrationthe resulting precipitate was collected by filtration
  4. washwashed with diethyl ether
  5. customdried in vacuo

Sources & evidence

ORD record
ord-d851c7c12fa94bbe9b868ee7cc649bdb
Source dataset
uspto-grants-2002_12
Patent number
US06492355B1

Reaction notes

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