1,4-Dioxane hydrochloride → HCID 136350898, compound

HRID 2217126Notes

Reaction equation

HRID 2217126 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]([NH:16][CH2:17][C:18]2[CH:40]=[CH:39][C:21]([C:22]([N:24]3[C:30]4[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=4[NH:28][C:27]4[N:35]([CH3:38])[N:36]=[CH:37][C:26]=4[CH2:25]3)=[O:23])=[CH:20][C:19]=2[CH3:41])=[O:15])[CH2:10][CH2:9]1)=O)(C)(C)C.[ClH:42].O1CCOCC1>>[ClH:42].[CH3:38][N:35]1[C:27]2[NH:28][C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[N:24]([C:22](=[O:23])[C:21]3[CH:39]=[CH:40][C:18]([CH2:17][NH:16][C:14]([N:11]4[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]4)=[O:15])=[C:19]([CH3:41])[CH:20]=3)[CH2:25][C:26]=2[CH:37]=[N:36]1

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 136355248HCID 136355248, compound

Product 1

HCID 136350898HCID 136350898, compound

Procedure

A solution of 5-(4-(4-(tert-butyloxycarbonyl)piperazine-1-carbonylaminomethyl)-3-methylbenzoyl)-1-methyl-4,10-dihydropyrazolo[5,4-b][1,5]benzodiazepine (160 mg, 0.29 mmol) in 4N HCl/dioxan (15 ml) was stirred at room temperature for 30 min then concentrated in vacuo. The residue was azeotroped with diethyl ether to give a white solid identified as 1-methyl-5-(3-methyl-4-(piperazine-1-carbonylaminomethyl)-benzoyl)-4,10-dihydropyrazolo[5,4-b][1,5]hydrochloride (130 mg, 90%).

Workup

  1. concentrationthen concentrated in vacuo
  2. customThe residue was azeotroped with diethyl ether
  3. customto give a white solid

Sources & evidence

ORD record
ord-f6955355d6174f219b2218f96e200793
Source dataset
uspto-grants-2008_08
Patent number
US07407949B2

Reaction notes

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