Carbon Disulfide → 2,4-Dichloro-alpha-(nitromethyl)benzyl dimethyldithiocarbamate

HRID 26139

반응식

HRID 26139 반응식
[Cl:1][C:2]1[CH:12]=[C:11]([Cl:13])[CH:10]=[CH:9][C:3]=1[CH:4]=[CH:5][N+:6]([O-:8])=[O:7].[CH3:14][N:15]([CH3:19])[C:16](=[S:18])[S-:17].C[NH2+]C.C(=S)=S>CO>[CH3:14][N:15]([CH3:19])[C:16](=[S:17])[S:18][CH:4]([CH2:5][N+:6]([O-:8])=[O:7])[C:3]1[CH:9]=[CH:10][C:11]([Cl:13])=[CH:12][C:2]=1[Cl:1]

참가 물질

5

반응물 3

HCID 6348Carbon DisulfideHCID 11728Dimethyldithiocarbamic acid, dimethylamineHCID 2558822,4-Dichloronitrostyrene

생성물 1

HCID 139566472,4-Dichloro-alpha-(nitromethyl)benzyl dimethyldithiocarbamate

시약·촉매·용매 1

HCID 887Methanol용매

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.

후처리

  1. customThe temperature of the resulting reaction
  2. customwas 16-32° C
  3. filtrationthe precipitated product was filtered off
  4. washwashed with cold methanol
  5. customdried in air
  6. customRecrystallization
  7. temperaturewithout heating
  8. dissolutionby dissolving the sample in acetone
  9. additionadding absolute ethanol

출처 및 근거

ORD 기록
ord-38ec2162fd244974ae314fd06409bdc0
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04148795

연결된 노트

불러오는 중…