Methanesulfonyl chloride → HCID 20039838, compound

HRID 1762836Notes

Reaction equation

HRID 1762836 reaction equation
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[NH2:6][C:7]1[CH:12]=[CH:11][C:10]([CH:13]2[CH2:18][CH2:17][N:16]([C:19]3[CH:24]=[CH:23][N:22]=[CH:21][CH:20]=3)[CH2:15][CH2:14]2)=[CH:9][CH:8]=1>N1C=CC=CC=1>[N:22]1[CH:21]=[CH:20][C:19]([N:16]2[CH2:17][CH2:18][CH:13]([C:10]3[CH:9]=[CH:8][C:7]([NH:6][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:12][CH:11]=3)[CH2:14][CH2:15]2)=[CH:24][CH:23]=1

Participants

4

Reactant 2

HCID 31297Methanesulfonyl chlorideHCID 20039823HCID 20039823, compound

Product 1

HCID 20039838HCID 20039838, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

Methanesulphonyl chloride (0.076 g) was added dropwise to a stirred solution of the product from part (ii) above (0.152 g) in pyridine (5.0 ml) at 0°. The mixture was stirred at room temperature for 3 hours and then evaporated. The residue was dissolved in water and an excess of solid sodium bicarbonate was added. The solid was filtered off, washed with water, dried and crystallised from methanol/ethyl acetate to give the title compound, (0.065 g), m.p. 269°-271° (with decomp).

Workup

  1. customevaporated
  2. dissolutionThe residue was dissolved in water
  3. additionan excess of solid sodium bicarbonate was added
  4. filtrationThe solid was filtered off
  5. washwashed with water
  6. customdried
  7. customcrystallised from methanol/ethyl acetate

Sources & evidence

ORD record
ord-16b009c7ad974ebba1d4a58c7257be05
Source dataset
uspto-grants-1989_05
Patent number
US04835165

Reaction notes

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