Toluene → N-(5-ethyl-1,3,4-thiadiazol-2-yl)butanamide

HRID 2256201노트

반응식

HRID 2256201 반응식
[NH2:1][C:2]1[S:3][C:4]([CH2:7][CH3:8])=[N:5][N:6]=1.C1(C)C=CC=CC=1.[C:16](Cl)(=[O:20])[CH2:17][CH2:18][CH3:19].C(=O)(O)[O-].[Na+]>C(OCC)(=O)C.C(N(CC)CC)C>[C:16]([NH:1][C:2]1[S:3][C:4]([CH2:7][CH3:8])=[N:5][N:6]=1)(=[O:20])[CH2:17][CH2:18][CH3:19]

참가 물질

7

반응물 4

HCID 1140TolueneHCID 8855Butyryl chlorideHCID 264442-Amino-5-ethyl-1,3,4-thiadiazoleHCID 516892Sodium Bicarbonate

생성물 1

HCID 693955N-(5-ethyl-1,3,4-thiadiazol-2-yl)butanamide수율 80.4%

시약·촉매·용매 2

HCID 8471Triethylamine용매HCID 8857Ethyl Acetate용매

실험 절차

2-Amino-5-ethyl-1,3,4-thiadiazole (0.5 g) was added to a mixture of toluene (5 ml) and triethylamine (0.4 g). With stirring, butyryl chloride (0.5 g) was added to the suspension at room temperature. After stirring for 2 hours, aqueous sodium bicarbonate solution and ethyl acetate were added to the reaction mixture. The organic layer was separated and washed with water several times. The precipitated crystals and the organic layer were combined and the solvent was concentrated to 5 ml. The precipitated crystals were filtrated and dried. The title compound (0.62 g) was obtained.

후처리

  1. stirringAfter stirring for 2 hours
  2. customThe organic layer was separated
  3. washwashed with water several times
  4. concentrationthe solvent was concentrated to 5 ml
  5. filtrationThe precipitated crystals were filtrated
  6. customdried

출처 및 근거

ORD 기록
ord-3677fff9712043b1a5b3ea709ac8e1e9
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05654322

반응 노트

불러오는 중…