Hydrochloric Acid → HCID 9987693, compound

HRID 736935Notes

Reaction equation

HRID 736935 reaction equation
O.[OH-].[Li+].C([O:6][C:7](=[O:58])[CH2:8][N:9]1[CH2:14][CH2:13][CH:12]([CH:15]2[CH2:20][CH2:19][N:18]([C:21](=[O:57])[C@H:22]([NH:36][C:37]([N:39]3[CH2:44][CH2:43][CH:42]([N:45]4[CH2:51][CH2:50][C:49]5[CH:52]=[CH:53][CH:54]=[CH:55][C:48]=5[NH:47][C:46]4=[O:56])[CH2:41][CH2:40]3)=[O:38])[CH2:23][C:24]3[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[C:27]([NH2:34])=[C:26]([Cl:35])[CH:25]=3)[CH2:17][CH2:16]2)[CH2:11][CH2:10]1)C.Cl>O.C1COCC1>[NH2:34][C:27]1[C:28]([C:30]([F:32])([F:31])[F:33])=[CH:29][C:24]([CH2:23][C@@H:22]([NH:36][C:37]([N:39]2[CH2:40][CH2:41][CH:42]([N:45]3[CH2:51][CH2:50][C:49]4[CH:52]=[CH:53][CH:54]=[CH:55][C:48]=4[NH:47][C:46]3=[O:56])[CH2:43][CH2:44]2)=[O:38])[C:21]([N:18]2[CH2:17][CH2:16][CH:15]([CH:12]3[CH2:13][CH2:14][N:9]([CH2:8][C:7]([OH:58])=[O:6])[CH2:10][CH2:11]3)[CH2:20][CH2:19]2)=[O:57])=[CH:25][C:26]=1[Cl:35]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 10056085HCID 10056085, compound

Product 1

HCID 9987693HCID 9987693, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of 20.1 mg (0.47 mmol) lithium hydroxide hydrate in 10 mL water was added to a solution of 250 mg (0.32 mmol) ethyl[1′-((R)-3-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-{[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-carbonyl]-amino}-propionyl)-4,4′-bipiperidinyl-1-yl]-acetate (Example 7.5) in 5 mL THF and the reaction mixture was stirred for 2 h at RT. 0.5 mL 1 M HCl were added, the substance precipitated was filtered off and dried at 50° C. The crude product was purified by HPLC.

Workup

  1. customthe substance precipitated
  2. filtrationwas filtered off
  3. customdried at 50° C
  4. customThe crude product was purified by HPLC

Sources & evidence

ORD record
ord-1679ef8b1b644dffbdabeeee3c1c6058
Source dataset
uspto-grants-2009_09
Patent number
US07595312B2

Reaction notes

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