Methyl iodide → Methyl 2-acetamidoethyldithiocarbamate

HRID 46597

반응식

HRID 46597 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 ml.) was added which again produced an exothermic reaction. After 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 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 1.75 hours the reaction mixture was evaporated to dryness
  6. dissolutionthe solid residue was dissolved in 200 ml
  7. extractionThe aqueous solution was extracted twice with 250 ml
  8. dry with materialdried (MgSO4)
  9. customevaporated to dryness

출처 및 근거

ORD 기록
ord-a2ddc4c0581344d993dfba587661d785
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04174323

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