Carbon Disulfide → HCID 86224690, 화합물

HRID 1863937노트

반응식

HRID 1863937 반응식
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

참가 물질

8

반응물 4

HCID 6348Carbon DisulfideHCID 10928Ethyl chloroformateHCID 14798Sodium HydroxideHCID 53407543HCID 53407543, 화합물

생성물 1

HCID 86224690HCID 86224690, 화합물

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-91b1f9edb73148b19811eb9c9c5abf0b
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07625888B2

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