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Triethylamine → HCID 20354904, 화합물

HRID 371571
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반응식

HRID 371571 반응식
[CH2:1]([N:4]([CH2:8][CH:9]=[CH2:10])[C:5](Cl)=[O:6])[CH:2]=[CH2:3].[CH2:11]([S:13][C:14]1[N:18]=[CH:17][NH:16][N:15]=1)[CH3:12].C(N(CC)CC)C>O1CCCC1>[CH2:1]([N:4]([CH2:8][CH:9]=[CH2:10])[C:5]([N:16]1[CH:17]=[N:18][C:14]([S:13][CH2:11][CH3:12])=[N:15]1)=[O:6])[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 3449313Diallylcarbamyl chlorideHCID 178477350HCID 178477350, 화합물

생성물 1

HCID 20354904HCID 20354904, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Diallylcarbamoyl chloride (8 g.) was added to a solution of 7.1 g. 3-ethylthio-1,2,4-triazole and 8 ml. dry triethylamine in 50 ml. dry tetrahydrofuran and the mixture refluxed for 4 hours under anhydrous conditions. The cooled reaction mixture was diluted with 100 ml. toluene and washed, firstly with 1N aqueous sodium hydroxide and then with water. The resulting solution was dried over anhydrous sodium sulphate and distilled under reduced pressure to remove the solvent and give 1-diallylcarbamoyl-3-ethylthio-1,2,4-triazole, b.p. 120° - 122° C./0.1 mm. (97.1% 1-isomer by GLC assay).

후처리

  1. customThe cooled reaction mixture
  2. additionwas diluted with 100 ml
  3. washtoluene and washed, firstly with 1N aqueous sodium hydroxide
  4. dry with materialThe resulting solution was dried over anhydrous sodium sulphate
  5. distillationdistilled under reduced pressure
  6. customto remove the solvent

출처 및 근거

ORD 기록
ord-af223ac949d34d97894988feb7b553a2
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087269

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