Ethyl vinyl ether → HCID 57434727, 화합물

HRID 1363068노트

반응식

HRID 1363068 반응식
[Br:1][C:2]1[C:6]([CH:7]=[O:8])=[C:5]([Br:9])[NH:4][N:3]=1.[CH:10]([O:12][CH2:13][CH3:14])=[CH2:11]>Cl.C1(C)C=CC=CC=1>[Br:1][C:2]1[C:6]([CH:7]=[O:8])=[C:5]([Br:9])[N:4]([CH:10]([O:12][CH2:13][CH3:14])[CH3:11])[N:3]=1

참가 물질

5

반응물 2

HCID 8023Ethyl vinyl ether2회HCID 574347263,5-dibromo-1H-pyrazole-4-carbaldehyde

생성물 1

HCID 57434727HCID 57434727, 화합물수율 92.7%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 1140Toluene용매2회

실험 절차

1 g (3.94 mmol) of 3,5-dibromo-1H-pyrazole-4-carboxaldehyde, 1.5 cm3 (16 mmol) of ethyl vinyl ether and 3 drops of 12N concentrated hydrochloric acid are introduced with stirring into 30 cm3 of toluene at a temperature in the region of 20° C. The reaction mixture is stirred for 15 hours at a temperature in the region of 20° C., 1.5 cm3 (16 mmol) of ethyl vinyl ether are then run in and stirring is continued for 15 hours at a temperature in the region of 20° C. The reaction mixture is then diluted with 20 cm3 of toluene and washed with twice 30 cm3 of saturated sodium hydrogen carbonate solution. The organic phase is dried over magnesium sulfate and concentrated to dryness under reduced pressure (2.7 kPa) to give 1.19 g of 3,5-dibromo-1-(1-ethoxyethyl)-1H-pyrazole-4-carboxaldehyde in the form of a yellow oil. 1H NMR spectrum (300 MHz, (CD3)2SO-d6, δ in ppm): 1.10 (t, J=7.5 Hz: 3H); 1.64 (d, J=6.5 Hz: 3H); 3.31 (mt: 1H); 3.51 (mt: 1H); 5.88 (q, J=6.5 Hz: 1H); 9.73 (s: 1H).

후처리

  1. washwashed with twice 30 cm3 of saturated sodium hydrogen carbonate solution
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

출처 및 근거

ORD 기록
ord-993ad3cbdd0543e9a06d82fa79efb56b
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07884123B2

반응 노트

불러오는 중…