Hydrochloric Acid → HCID 9911003, compound

HRID 2298046Notes

Reaction equation

HRID 2298046 reaction equation
C[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][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].[ClH:36]>CO.O1CCOCC1>[ClH:36].[Cl:36][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][C:26]12[CH2:33][CH:32]3[CH2:31][CH:30]([CH2:29][CH:28]([CH2:34]3)[CH2:27]1)[CH2:35]2)=[O:23]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 86758642HCID 86758642, compound

Product 1

HCID 9911003HCID 9911003, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 312751,4-DioxaneSolvent

Procedure

Hexahydro-4-[4-methyl-3-[[(tricyclo[3.3.1.13,7]dec-1-ylmethyl)amino]carbonyl]-phenyl]-1H-1,4-diazepine-1-carboxylic acid, 1,1-dimethylethyl ester (from Example 5c) was dissolved in methanol (5 ml) and hydrochloric acid (0.5 ml of a 4N solution in dioxane) was added. After stirring at room temperature for 14 h, the mixture was evaporated to ⅔ original volume under reduced pressure. Diethyl ether was gradually added to the solution and the resulting precipitate collected by filtration, washed with diethyl ether and dried in vacuo to afford the title compound as a solid (0.027 g)

Workup

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

Sources & evidence

ORD record
ord-9e369be39f2040f383b51049a3e5b01c
Source dataset
uspto-grants-2002_12
Patent number
US06492355B1

Reaction notes

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