Triethylamine → HCID 15231190, compound

HRID 2353430Notes

Reaction equation

HRID 2353430 reaction equation
[CH3:1][C:2]1[S:3][CH:4]2[CH2:9][N:8]([S:10]([C:13]3[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=3)(=[O:12])=[O:11])[CH2:7][C:5]2(O)[N:6]=1.CS(Cl)(=O)=O.C(N(CC)CC)C>ClCCl>[CH3:1][C:2]1[S:3][C:4]2[CH2:9][N:8]([S:10]([C:13]3[CH:18]=[CH:17][C:16]([CH3:19])=[CH:15][CH:14]=3)(=[O:11])=[O:12])[CH2:7][C:5]=2[N:6]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 15231189HCID 15231189, compound

Product 1

HCID 15231190HCID 15231190, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of the product from Step A (150 mg) in dichloromethane (2 mL) was added methanesulfonyl chloride (0.074 mL) at 0° C. followed by triethylamine (0.67 mL). After 15 min the reaction mixture was warmed to ambient temperature and stirred for 45 min. The mixture was concentrated in vacuo and purified by preparative thin layer chromatography using an Analtech® 1500 micron plate (8% ethyl acetate/dichloromethane) to give the title compound as a white solid. LC/MS 295.2 (M+1).

Workup

  1. concentrationThe mixture was concentrated in vacuo
  2. custompurified by preparative thin layer chromatography

Sources & evidence

ORD record
ord-1b8e2c83d89d435786b038af22c1bd11
Source dataset
uspto-grants-2010_07
Patent number
US07750034B2

Reaction notes

Loading…