반응 #54417

반응 방정식

2,4-Dichloro-β-nitrostyrene

dimethylammonium dimethyldithiocarbamate

carbon disulfide

→

2,4-dichloro-α-(nitromethyl)-benzyl dimethyldithiocarbamate

용매

methanol

반응 조건

후처리

1. 1
   기타The temperature of the resulting reaction
2. 2
   기타was 16-32° C
3. 3
   여과the precipitated product was filtered off
4. 4
   세척washed with cold methanol
5. 5
   기타dried in air
6. 6
   기타Recrystallization
7. 7
   온도without heating
8. 8
   workup.DISSOLUTIONby dissolving the sample in acetone
9. 9
   workup.ADDITIONadding absolute ethanol

실험 절차

2,4-Dichloro-β-nitrostyrene (6.6 grams, 0.030 mole) was added to a stirred solution of dimethylammonium dimethyldithiocarbamate (5.1 grams, 0.030 mole) and carbon disulfide (1.8 ml., 0.030 mole) in methanol (30 ml.). The temperature of the resulting reaction was 16-32° C. After two hours at room temperature, the precipitated product was filtered off, washed with cold methanol, and dried in air. Recrystallization without heating was accomplished by dissolving the sample in acetone and then adding absolute ethanol to give 2,4-dichloro-α-(nitromethyl)-benzyl dimethyldithiocarbamate melting at 127° C.-128° C.

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