Benzaldehyde → alpha-(Nitromethyl)benzyl dimethyldithiocarbamate

HRID 26135

反応式

HRID 26135 の反応式
[CH3:1][N:2]([CH3:6])[C:3](=[S:5])[S-:4].C[NH2+]C.C(=S)=S.[CH:13](=O)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[N+:21]([CH3:24])([O-:23])=[O:22]>C(O)C>[CH3:1][N:2]([CH3:6])[C:3](=[S:4])[S:5][CH:13]([CH2:24][N+:21]([O-:23])=[O:22])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

参加物

6

反応物 4

HCID 240BenzaldehydeHCID 6348Carbon DisulfideHCID 6375NitromethaneHCID 11728Dimethyldithiocarbamic acid, dimethylamine

生成物 1

HCID 21324598alpha-(Nitromethyl)benzyl dimethyldithiocarbamate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of dimethylammonium dimethyldithiocarbamate (16.6 grams, 0.10 mole), carbon disulfide (7.6 grams, 0.10 mole), benzaldehyde (21.2 grams, 0.20 mole) and nitromethane (9.2 grams, 0.15 mole) in 95% ethanol (50 ml.) was allowed to stand at 23° C. for several days. The resulting precipitate was filtered off, washed with cold 95% ethanol, and dried in air. The solid product, which melted at 101° C.-102° C., was recrystallized from 2-propanol to give α-(nitromethyl)benzyl dimethyldithiocarbamate melting at 105° C.-106° C. The structure was determined from infrared and nuclear magnetic resonance spectra and elemental analysis.

後処理

  1. waitto stand at 23° C. for several days
  2. filtrationThe resulting precipitate was filtered off
  3. washwashed with cold 95% ethanol
  4. customdried in air
  5. customThe solid product, which melted at 101° C.-102° C., was recrystallized from 2-propanol

出典と根拠

ORDレコード
ord-b12af338d5e445109bf46b1ee5d17697
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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