Dimethylamine → HCID 54025393, compound

HRID 1278259Notes

Reaction equation

HRID 1278259 reaction equation
[CH3:1][NH:2][CH3:3].O1[CH2:8][CH2:7][CH2:6][CH2:5]1.[C:9](=[S:11])=[S:10].C(Cl)C=CC>O>[CH2:5]([S:10][C:9](=[S:11])[N:2]([CH3:3])[CH3:1])[CH:6]=[CH:7][CH3:8]

Participants

6

Procedure

12.0 Grams of a 50% dimethylamine aqueous solution was added to 30 ml of tetrahydrofuran, and to this mixture being maintained a temperature at 0°-5° C., was added dropwise 5.0 gr of carbon disulfide under agitation over the period of 30 minutes. Thereafter, the reaction mixture was maintained at a room temperature and further 5.4 gr of crotyl chloride was added dropwise thereto over the period of 30 minutes, and this was followed by 3-hour agitation at the same temperature to complete the reaction. The reaction mixture was poured into water and the separated organic substance was extracted twice with 30 ml of toluene, washed with diluted hydrochloric acid and further washed with water, and then toluene was removed by distillation to obtain 10.2 gr of the desired product having the following physical properties.

Workup

  1. temperatureto this mixture being maintained a temperature at 0°-5° C.
  2. customthe reaction
  3. extractionthe separated organic substance was extracted twice with 30 ml of toluene
  4. washwashed with diluted hydrochloric acid
  5. washfurther washed with water
  6. customtoluene was removed by distillation

Sources & evidence

ORD record
ord-757ce8f4edd445488da763c74832f6cc
Source dataset
uspto-grants-1981_07
Patent number
US04281016

Reaction notes

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