Methyl iodide → Methyl 2-acetamidoethyldithiocarbamate

HRID 839595ノート

反応式

HRID 839595 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 20501582Methyl 2-acetamidoethyldithiocarbamate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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 was cooled to ambient temperature over a 1.5 hour period. Methyl iodide (28.4 g., 0.20 mol.) 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.

後処理

  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

出典と根拠

ORDレコード
ord-f77a2c464d3e480bb4cf1f5ecb8a5d7e
出典データセット
uspto-grants-1978_06
特許番号
US04096256

反応ノート

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