Triethylamine → HCID 20354889, 화합물

HRID 371566노트

반응식

HRID 371566 반응식
[CH2:1]([N:4]([CH2:8][CH2:9][CH3:10])[C:5](Cl)=[O:6])[CH2:2][CH3:3].[CH3:11][S:12]([C:15]1[N:19]=[CH:18][NH:17][N:16]=1)(=[O:14])=[O:13].C(N(CC)CC)C>O1CCCC1>[CH2:1]([N:4]([CH2:8][CH2:9][CH3:10])[C:5]([N:17]1[CH:18]=[N:19][C:15]([S:12]([CH3:11])(=[O:14])=[O:13])=[N:16]1)=[O:6])[CH2:2][CH3:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 3015348Dipropylcarbamoyl chlorideHCID 178504852HCID 178504852, 화합물

생성물 1

HCID 20354889HCID 20354889, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Dipropylcarbamoyl chloride (5.5 g.) was added to a solution of 4.4 g. 3-methylsulphonyl-1,2,4-triazole and 6 ml. dry triethylamine in 25 ml. dry tetrahydrofuran and the resulting mixture refluxed for 2.5 hours under anhydrous conditions. The cooled reaction mixture was filtered to remove triethylamine hydrochloride and the filtrate poured with stirring into 150 ml. ice-cold 0.1N aqueous sodium hydroxide. The precipitated product was collected by filtration, washed with ice-cold water, dried, and crystallized twice from toluene to give 1-dipropylcarbamoyl-3-methylsulphonyl-1,2,4-triazole, m.p. 94° C. Elemental analysis satisfactory.

후처리

  1. customThe cooled reaction mixture
  2. filtrationwas filtered
  3. customto remove triethylamine hydrochloride
  4. additionthe filtrate poured
  5. filtrationThe precipitated product was collected by filtration
  6. washwashed with ice-cold water
  7. customdried
  8. customcrystallized twice from toluene

출처 및 근거

ORD 기록
ord-cb70e4162be44d7cb84dcbf826d08c59
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04087269

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