Methylamine → HCID 21545015, compound

HRID 1605800Notes

Reaction equation

HRID 1605800 reaction equation
Cl[CH2:2][CH:3]1[S:9][CH2:8][CH2:7][CH2:6][CH2:5][S:4]1.[OH-].[Na+].[CH3:12][NH2:13]>>[S:4]1[CH2:5][CH2:6][CH2:7][CH2:8][S:9][CH:3]1[CH2:2][NH:13][CH3:12]

Participants

4

Reactant 3

HCID 6329MethylamineHCID 14798Sodium HydroxideHCID 21545027HCID 21545027, compound

Product 1

HCID 21545015HCID 21545015, compound

Procedure

A 40% by weight aqueous solution of methylamine (100 ml) and 2-chloromethyl-1,3-dithiepane (50 grams) are charged into a glass reaction vessel equipped with a mechanical stirrer. The reaction mixture is stirred for a period of about 18 hours. After this time sodium hydroxide (18 grams) is added with stirring over a period of about 3 hours. Stirring is then continued for an additional period of about 16 hours. The organic phase of the reaction mixture is then separated, is washed with aqueous potasssium carbonate and dried over anhydrous magnesium sulfate. The dried product is then distilled under reduced pressure to yield the desired product N-(1,3-dithiepan-2-ylmethyl)-N-methylamine.

Workup

  1. customequipped with a mechanical stirrer
  2. stirringwith stirring over a period of about 3 hours
  3. stirringStirring
  4. waitis then continued for an additional period of about 16 hours
  5. customThe organic phase of the reaction mixture is then separated
  6. washis washed with aqueous potasssium carbonate
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe dried product is then distilled under reduced pressure

Sources & evidence

ORD record
ord-41e82b9e59284d889495bae0eea340c3
Source dataset
uspto-grants-1976_04
Patent number
US03951640

Reaction notes

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