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

HRID 26139

反応式

HRID 26139 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-38ec2162fd244974ae314fd06409bdc0
出典データセット
uspto-grants-1979_04
特許番号
US04148795

関連ノート

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