Methyl iodide → Methyl 2-acetamidoethyldithiocarbamate

HRID 866876

반응식

HRID 866876 반응식
[NH2:1][CH2:2][CH2:3][NH:4][C:5](=[O:7])[CH3:6].C(N(CC)CC)C.[C:15](=[S:17])=[S:16].[CH3:18]I>C(O)C>[C:5]([NH:4][CH2:3][CH2:2][NH:1][C:15](=[S:17])[S:16][CH3:18])(=[O:7])[CH3:6]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 66082N-(2-aminoethyl)acetamide

생성물 1

HCID 20501582Methyl 2-acetamidoethyldithiocarbamate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 20.4 g (0.20 mol) of N-(2-aminoethyl)acetamide in 200 ml of 95% ethanol was added 27.9 ml (0.20 mol) of triethylamine and 12.0 ml (0.20 mol) of carbon disulfide. The exothermic reaction reached reflux and then cooled to ambient temperature over a 1.5 hour period. Methyl iodide (28.4 g, 0.20 mol) was then added which again produced an exothermic reaction. After an additional 1.75 hours the reaction mixture was evaporated to dryness and the solid residue was dissolved in 200 ml of water. The aqueous solution was extracted twice with 250 ml portions of ethyl acetate. The extracts were combined, shaken with solid sodium thiosulfate, dried (MgSO4) and evaporated to dryness to give methyl 2-acetamidoethyldithiocarbamate.

후처리

  1. customThe exothermic reaction
  2. temperaturereached reflux
  3. customagain produced
  4. customan exothermic reaction
  5. customAfter an additional 1.75 hours the reaction mixture was evaporated to dryness
  6. dissolutionthe solid residue was dissolved in 200 ml of water
  7. extractionThe aqueous solution was extracted twice with 250 ml portions of ethyl acetate
  8. dry with materialdried (MgSO4)
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-7a65c47ef51f4ba681707a32a457aae0
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04101656

연결된 노트

불러오는 중…