Carbon Disulfide → HCID 86224690、化合物

HRID 1863937ノート

反応式

HRID 1863937 の反応式
Cl.Cl.[CH3:3][C:4]1[NH:8][N:7]=[C:6]([CH2:9][CH2:10][NH2:11])[N:5]=1.[OH-].[Na+].[C:14](=S)=[S:15].ClC(OCC)=O>O.C(O)C.C(O)(=O)C>[CH3:3][C:4]1[N:5]=[C:6]2[N:7]([C:14](=[S:15])[NH:11][CH2:10][CH2:9]2)[N:8]=1

参加物

8

反応物 4

HCID 6348Carbon DisulfideHCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 53407543HCID 53407543、化合物

生成物 1

HCID 86224690HCID 86224690、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of 1.99 g (10 mmol) of 2-(5-methyl-1,2,4-triazol-3-yl)ethanamine dihydrochloride in a mixture of 13 mL of water and 7 mL (35 mmol) of 5N sodium hydroxide aqueous solution was stirred under nitrogen at room temperature as a solution of 5.4 mL of carbon disulfide in 30 mL of dry ethanol was added dropwise over about 30 minutes. After 5 h, the excess carbon disulfide was removed by rotary evaporation. The resulting solution was stirred under nitrogen at room temperature as 1.08 mL (1.23 g, 11 mmol) of ethyl chloroformate was added dropwise over about 10 minutes. Stirring at room temperature was continued overnight. The solution was partially concentrated to remove the ethanol, resulting in precipitation. The pH was made slightly acidic by addition of acetic acid. Then the solid was collected on a filter, washed with a small volume of water, and dried to give the title compound as a solid. LC-MS 169 (M+1).

後処理

  1. additionwas added dropwise over about 30 minutes
  2. customthe excess carbon disulfide was removed by rotary evaporation
  3. additionwas added dropwise over about 10 minutes
  4. waitwas continued overnight
  5. concentrationThe solution was partially concentrated
  6. customto remove the ethanol
  7. customresulting in precipitation
  8. customThen the solid was collected on a filter
  9. washwashed with a small volume of water
  10. customdried

出典と根拠

ORDレコード
ord-91b1f9edb73148b19811eb9c9c5abf0b
出典データセット
uspto-grants-2009_12
特許番号
US07625888B2

反応ノート

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