Dimethylformamide → HCID 178418411, 화합물

HRID 2690

반응식

HRID 2690 반응식
Br[CH2:2][CH2:3]Br.[N-:5]=[N+:6]=[N-:7].[Na+].[N-]=[N+:10]=[N-:11].[Li][CH3:13].C[N:15]([CH:17]=O)C>>[CH3:13][NH:5][N:6]=[N:7][CH2:2][CH2:3][N:10]=[N:11][NH:15][CH3:17]

참가 물질

6

반응물 5

HCID 6228DimethylformamideHCID 78391,2-DibromoethaneHCID 33557Sodium AzideHCID 33558AzideHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 178418411HCID 178418411, 화합물수율 32%

반응 조건

온도
50 °C

실험 절차

A flask is charged with 5.0 g (27 mmole) of 1,2-dibromoethane, 3.8 g (58 mmole) of sodium azide, and 50 ml of DMF. The mixture is heated at 50° C. with stirring under argon overnight. The mixture is worked up as described above, except that the azide solution is not evaporated down totally. When about 30 ml of solution remains the mixture is treated with 45 ml of a 1.3M solution of MeLi (58 mmole) as above. After 3 hr the reaction is worked up as described above, and a yellow solid is obtained. Crystallization from ether/petroleum ether affords 1.23 g (32% yield) of an off-white solid, mp 64°-6° C. Mass spectra (FAB) Calc (M+H) 145.1201, Found 145.1220±0.0015.

후처리

  1. customis not evaporated down totally
  2. waitAfter 3 hr the reaction is worked up
  3. customis obtained
  4. customCrystallization from ether/petroleum ether

출처 및 근거

ORD 기록
ord-1a927144cffe4757b1c0239ad6f9ed5a
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05731301

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