Triethylamine → HCID 20354889、化合物

HRID 1606054ノート

反応式

HRID 1606054 の反応式
[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]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 3015348Dipropylcarbamoyl chlorideHCID 178504852HCID 178504852、化合物

生成物 1

HCID 20354889HCID 20354889、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-47f8345df87048c78a38e5531afa370d
出典データセット
uspto-grants-1976_04
特許番号
US03952001

反応ノート

読み込み中…