Hydrochloric Acid → HCID 69592660, compound

HRID 1241608Notes

Reaction equation

HRID 1241608 reaction equation
[CH2:1]([N:3]([CH2:50][CH3:51])[CH2:4][CH2:5][N:6]([C:24]([CH2:26][N:27]1[CH:32]=[C:31]([CH2:33][C:34]2[CH:35]=[N:36][N:37]([CH3:39])[CH:38]=2)[C:30](=[O:40])[N:29]=[C:28]1[S:41][CH2:42][C:43]1[CH:48]=[CH:47][C:46]([F:49])=[CH:45][CH:44]=1)=[O:25])[CH2:7][C:8]1[CH:9]=[CH:10][C:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:23])([F:22])[F:21])=[CH:16][CH:15]=2)=[N:12][CH:13]=1)[CH3:2].[ClH:52].CCOCC>ClCCl>[ClH:52].[CH2:50]([N:3]([CH2:1][CH3:2])[CH2:4][CH2:5][N:6]([C:24]([CH2:26][N:27]1[CH:32]=[C:31]([CH2:33][C:34]2[CH:35]=[N:36][N:37]([CH3:39])[CH:38]=2)[C:30](=[O:40])[N:29]=[C:28]1[S:41][CH2:42][C:43]1[CH:48]=[CH:47][C:46]([F:49])=[CH:45][CH:44]=1)=[O:25])[CH2:7][C:8]1[CH:9]=[CH:10][C:11]([C:14]2[CH:19]=[CH:18][C:17]([C:20]([F:21])([F:22])[F:23])=[CH:16][CH:15]=2)=[N:12][CH:13]=1)[CH3:51]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 23395770HCID 23395770, compound

Product 1

HCID 69592660HCID 69592660, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

The free base from Example 17 (0.373 g, 1 equiv) was dissolved in dichloromethane (10 ml), and a solution of hydrogen chloride in ether (0.517 ml, 1.0M solution, 1 equiv) was added dropwise with stirring. The solvent was removed in vacuo, and the residue triturated with ether to obtain a white solid (0.362 g). 1H-NMR (DMSO, ca. 60:40 rotamer mixture) δ 1.1–1.3 (6H,m), 3.77 (3H,s), 4.38/4.43 (2H,s), 4.65/4.76 (2H,s), 5.00/5.08 (2H,s), 7.10 (2H,m), 7.25 (1H,m), 7.3–7.5 (4H,m) 7.78 (1H,m), 7.87 (2H,d), 7.97/8.06 (1H,d), 8.28 (2H,d), 8.61/8.70 (1H,m); MS (APCI+) found (M+1)=722; C37H39F4N7O2S requires 721.

Workup

  1. customThe solvent was removed in vacuo
  2. customthe residue triturated with ether

Sources & evidence

ORD record
ord-018e0ac2ab3148ed966d3c162bee8120
Source dataset
uspto-grants-2006_10
Patent number
US07115616B2

Reaction notes

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