Benzaldehyde → alpha-(Nitromethyl)benzyl dimethyldithiocarbamate

HRID 26135

반응식

HRID 26135 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 21324598alpha-(Nitromethyl)benzyl dimethyldithiocarbamate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b12af338d5e445109bf46b1ee5d17697
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04148795

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