Methylamine → HCID 13983539, compound

HRID 1084937Notes

Reaction equation

HRID 1084937 reaction equation
[CH3:1][NH2:2].[Br:3][C:4]1[C:13]([S:14](Cl)(=[O:16])=[O:15])=[CH:12][C:11]([C:18]([OH:20])=[O:19])=[C:10]2[C:5]=1[CH2:6][CH2:7][CH2:8][O:9]2.[OH-].[Na+]>O>[Br:3][C:4]1[C:13]([S:14](=[O:16])(=[O:15])[NH:2][CH3:1])=[CH:12][C:11]([C:18]([OH:20])=[O:19])=[C:10]2[C:5]=1[CH2:6][CH2:7][CH2:8][O:9]2

Participants

5

Reactant 3

HCID 6329MethylamineHCID 14798Sodium HydroxideHCID 20062867HCID 20062867, compound

Product 1

HCID 13983539HCID 13983539, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
0 °C

Procedure

70 g of methylamine in a 40% aqueous solution and 70 ml of water were introduced into a 1-liter round-bottomed flask. The contents were cooled to 0° C. and 160 g of 5-bromo-6-chlorosulphonylchroman-8-carboxylic acid were added in 16 g portions, the introduction of each portion of acid being followed by the addition of 18 ml of a solution containing 90 ml of 30% sodium hydroxide in 90 ml of water. The temperature was maintained between 0° and 5° C. during the entire period of introduction and for a further period of one hour. The temperature was then allowed to rise. The solution obtained was taken up with 1 liter of water, filtered with charcoal and acidified with concentrated hydrochloric acid until a color change of Congo red was observed.

Workup

  1. temperatureThe temperature was maintained between 0° and 5° C. during the entire period of introduction and for a further period of one hour
  2. customThe solution obtained
  3. filtrationfiltered with charcoal

Sources & evidence

ORD record
ord-baa58c60bb47440a95d81fac1c13d264
Source dataset
uspto-grants-1991_04
Patent number
US05006570

Reaction notes

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