Hydrochloric Acid → HCID 69061225, compound

HRID 1869597Notes

Reaction equation

HRID 1869597 reaction equation
[N:1]1([C:7]([O:9][C@H:10]([CH2:37][C:38]2[CH:43]=[C:42]([CH3:44])[C:41]([OH:45])=[C:40]([CH3:46])[CH:39]=2)[C:11]([N:13]2[CH2:18][CH2:17][C:16]([N:25]3[CH2:31][CH2:30][C:29]4[CH:32]=[CH:33][CH:34]=[CH:35][C:28]=4[NH:27][C:26]3=[O:36])([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[CH2:15][CH2:14]2)=[O:12])=[O:8])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:47].C(OC)(C)(C)C>C(O)C>[ClH:47].[N:1]1([C:7]([O:9][C@H:10]([CH2:37][C:38]2[CH:43]=[C:42]([CH3:44])[C:41]([OH:45])=[C:40]([CH3:46])[CH:39]=2)[C:11]([N:13]2[CH2:14][CH2:15][C:16]([N:25]3[CH2:31][CH2:30][C:29]4[CH:32]=[CH:33][CH:34]=[CH:35][C:28]=4[NH:27][C:26]3=[O:36])([N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)[CH2:17][CH2:18]2)=[O:12])=[O:8])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 15413tert-Butyl methyl etherHCID 69058107HCID 69058107, compound

Product 1

HCID 69061225HCID 69061225, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

0.5 g (0.79 mmol) 4-(1,2,4,5-tetrahydro-2-oxo-3H-1,3-benzodiazepin-3-yl)-(1R)-1-[(4-hydroxy-3,5-dimethylphenyl)methyl]-2-[4-(4-morpholinyl)-1-piperidinyl]-2-oxoethyl 1-piperidinecarboxylate are dissolved in 5 ml of ethanol at ambient temperature and combined with 65.3 μl hydrochloric acid (37% in water). After 2 hours at ambient temperature tert-butylmethylether is added dropwise until turbidity sets in. After another 2 hours at ambient temperature the white precipitate formed is filtered off, washed with tert-butyl-methylether and dried for 12 hours at 40° C.

Workup

  1. customAfter another 2 hours at ambient temperature the white precipitate formed
  2. filtrationis filtered off
  3. washwashed with tert-butyl-methylether
  4. customdried for 12 hours at 40° C.

Sources & evidence

ORD record
ord-119ba473c66748f69fe30e4ac3495028
Source dataset
uspto-grants-2009_12
Patent number
US07638625B2

Reaction notes

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