Water → HCID 21094318, compound

HRID 1350078Notes

Reaction equation

HRID 1350078 reaction equation
[OH:1][CH2:2][CH:3]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[CH2:6][N:5]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:4]1.C(N(CC)CC)C.[CH3:29][S:30](Cl)(=[O:32])=[O:31].O>ClCCl>[CH3:14][O:13][C:10]1[CH:11]=[C:12]2[C:7](=[CH:8][CH:9]=1)[CH2:6][N:5]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:4][CH:3]2[CH2:2][O:1][S:30]([CH3:29])(=[O:32])=[O:31]

Participants

6

Reactant 4

HCID 962WaterHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 21094316HCID 21094316, compound

Product 1

HCID 21094318HCID 21094318, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Conditions

Temperature
0 °C

Procedure

The compound obtained in Step G (10.5 g; 36 mmol) is dissolved in 150 ml of dichloromethane and then triethylamine (8.5 ml) is added. The solution is cooled to 0° C. and methanesulphonyl choride (4.8 ml; 62 mmol) is added dropwise. The reaction mixture is stirred at ambient temperature for 2 hours and then poured into 150 ml of water. The solution is extracted with dichloromethane, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The title compound is purified by chromatography on silica gel.

Workup

  1. extractionThe solution is extracted with dichloromethane
  2. dry with materialdried over magnesium sulphate
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe title compound is purified by chromatography on silica gel

Sources & evidence

ORD record
ord-fca03856606c4d8dbfc42cbd148e16f4
Source dataset
uspto-grants-2007_05
Patent number
US07214689B2

Reaction notes

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