반응식
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[Cl-].[Li+].[N-:15]=[N+:16]=[N-:17].[Na+].[Br-].C([NH+](CC)CC)C.Cl>CN(C=O)C.O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:9]2[NH:17][N:16]=[N:15][N:10]=2)=[CH:11][CH:12]=1)([CH3:4])([CH3:2])[CH3:3]참가 물질
8
실험 절차
4.99 of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF were heated at 120° C. for 8 h in a 250 ml round-bottom flask fitted with a reflux condenser. After cooling to room temperature, 100 ml of water were added, and, in an ice bath, dilute hydrochloric acid was added until no more precipitate formed. The mixture was filtered with suction, and the precipitate was washed with water and dried. Recrystallization from ethanol/water produced 4.4 g of colorless crystals.
후처리
- customfitted with a reflux condenser
- customformed
- filtrationThe mixture was filtered with suction
- washthe precipitate was washed with water
- customdried
- customRecrystallization from ethanol/water
출처 및 근거
- ORD 기록
- ord-0561e6e8c8e64a3dac1e01782ec069c9
- 출처 데이터셋
- uspto-grants-2001_02
- 특허 번호
- US06187224B1
연결된 노트
불러오는 중…