Hydrogen Bromide → HCID 68825644, compound

HRID 1869600Notes

Reaction equation

HRID 1869600 reaction equation
[NH2:1][C:2]1[C:45]([C:46]([F:49])([F:48])[F:47])=[CH:44][C:5]([CH2:6][C@@H:7]([CH2:23][C:24]([N:26]2[CH2:31][CH2:30][CH:29]([N:32]3[CH2:38][CH2:37][C:36]4[CH:39]=[CH:40][CH:41]=[CH:42][C:35]=4[NH:34][C:33]3=[O:43])[CH2:28][CH2:27]2)=[O:25])[C:8]([N:10]2[CH2:15][CH2:14][CH:13]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][C:3]=1[Cl:50].[BrH:51]>C(O)(C)C>[OH2:9].[OH2:9].[OH2:9].[OH2:9].[OH2:9].[BrH:51].[NH2:1][C:2]1[C:45]([C:46]([F:48])([F:47])[F:49])=[CH:44][C:5]([CH2:6][C@@H:7]([CH2:23][C:24]([N:26]2[CH2:27][CH2:28][CH:29]([N:32]3[CH2:38][CH2:37][C:36]4[CH:39]=[CH:40][CH:41]=[CH:42][C:35]=4[NH:34][C:33]3=[O:43])[CH2:30][CH2:31]2)=[O:25])[C:8]([N:10]2[CH2:15][CH2:14][CH:13]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)[CH2:12][CH2:11]2)=[O:9])=[CH:4][C:3]=1[Cl:50]

Participants

4

Reactant 2

HCID 260Hydrogen BromideHCID 10327519HCID 10327519, compound

Product 1

HCID 68825644HCID 68825644, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Conditions

Temperature
4 °C

Procedure

2.0 g (2.6 mmol) (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-1-[4-(4-methyl-piperazin-1-yl)-piperidin-1-yl]-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butane-1,4-dione are dissolved in 20 ml isopropanol and at 50° C. combined with 0.6 ml hydrobromic acid (47% in water). The mixture is cooled to 4° C. within 30 minutes. The solid formed is filtered off, washed with 5 ml cold isopropanol and dried for 12 hours at 40° C.

Workup

  1. customThe solid formed
  2. filtrationis filtered off
  3. washwashed with 5 ml cold isopropanol
  4. customdried for 12 hours at 40° C.

Sources & evidence

ORD record
ord-6c1adfd3480c41099f2fbbf32f9b97cc
Source dataset
uspto-grants-2009_12
Patent number
US07638625B2

Reaction notes

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