Methanesulfonyl chloride → HCID 136128369, compound

HRID 220805Notes

Reaction equation

HRID 220805 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.[CH3:7][N:8]1[C:17]2[NH:16][C:15]3[CH:18]=[C:19]([CH3:22])[CH:20]=[CH:21][C:14]=3[N:13]([C:23]([CH:25]3[CH2:30][CH2:29][CH:28]([CH2:31][NH:32][C:33](=[O:41])[CH2:34][CH:35]4[CH2:40][CH2:39][NH:38][CH2:37][CH2:36]4)[CH2:27][CH2:26]3)=[O:24])[CH2:12][C:11]=2[CH:10]=[N:9]1>ClCCl.C(N(CC)CC)C>[CH3:7][N:8]1[C:17]2[NH:16][C:15]3[CH:18]=[C:19]([CH3:22])[CH:20]=[CH:21][C:14]=3[N:13]([C:23]([CH:25]3[CH2:26][CH2:27][CH:28]([CH2:31][NH:32][C:33](=[O:41])[CH2:34][CH:35]4[CH2:36][CH2:37][N:38]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:39][CH2:40]4)[CH2:29][CH2:30]3)=[O:24])[CH2:12][C:11]=2[CH:10]=[N:9]1

Participants

5

Reactant 2

HCID 31297Methanesulfonyl chlorideHCID 136346634HCID 136346634, compound

Product 1

HCID 136128369HCID 136128369, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolvent2×HCID 8471TriethylamineSolvent

Procedure

A solution of methanesulfonyl chloride (0.57 mg, 0.005 mmol) in dichloromethane (0.05 ml) was added to a solution of N-[4-(3,6-dimethyl-4,10-dihydro-3H-2,3,4,9-tetraaza-benzo[f]azulene-9-carbonyl)-cyclohexylmethyl]-2-piperidin-4-yl-acetamide hydrochloride from Example E17 (2.57 mg, 0.005 mmol) in dichloro-methane (0.05 ml) and triethylamine (0.0035 ml). The mixture was stirred at room temperature for 1 h then sol-vents were removed in vacuo to yield the title compound. (ESI)+: [M+H]+=557.4

Workup

  1. customthen sol-vents were removed in vacuo

Sources & evidence

ORD record
ord-8b3f9ad98f944fbeab77124132adad50
Source dataset
uspto-grants-2012_06
Patent number
US08202858B2

Reaction notes

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