Dimethylformamide → HCID 178418411、化合物

HRID 2690

反応式

HRID 2690 の反応式
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]

参加物

6

反応物 5

HCID 6228DimethylformamideHCID 78391,2-DibromoethaneHCID 33557Sodium AzideHCID 33558AzideHCID 178418348HCID 178418348、化合物

生成物 1

HCID 178418411HCID 178418411、化合物収率 32%

反応条件

温度
50 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-1a927144cffe4757b1c0239ad6f9ed5a
出典データセット
uspto-grants-1998_03
特許番号
US05731301

関連ノート

読み込み中…