1,2-Dichloroethane → HCID 66685531, 화합물

HRID 922248노트

반응식

HRID 922248 반응식
ClCCCl.[CH3:5][C:6]1[CH:10]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([N+:17]([O-:19])=[O:18])=[CH:13][CH:12]=2)[O:8][N:7]=1.[I:20]N1C(=O)CCC1=O.OS(O)(=O)=O>O>[I:20][C:10]1[C:6]([CH3:5])=[N:7][O:8][C:9]=1[C:11]1[CH:12]=[CH:13][C:14]([N+:17]([O-:19])=[O:18])=[CH:15][CH:16]=1

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 1118Sulfuric AcidHCID 120273N-IodosuccinimideHCID 37721263-Methyl-5-(4-nitrophenyl)isoxazole

생성물 1

HCID 66685531HCID 66685531, 화합물수율 97.7%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 100 mL RB flask fitted with magnetic stirrer was charged with 10 mL of 1,2-dichloroethane. To the stirring solution were added 3-methyl-5-(4-nitrophenyl)-1,2-oxazole (0.27 g, 1.30 mmol), N-iodosuccinimide (0.28 g, 1.24 mmol), followed by concentrated H2SO4 (0.2 mL) at 0° C. and stirred at room temperature for 4 h. The reaction mixture was poured into water (30 mL) and extracted with ethyl acetate (50 mL). The organic layer was washed with sodium thiosulphate solution (30 mL), water (30 mL) and saturated brine solution (10 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The product was obtained as yellow solid (0.40 g, yield: 93.7%). 1H NMR (300 MHz, CDCl3): δ 8.29-8.32 (dd, 2H), 8.18-8.21 (dd, 2H), 2.33 (s, 3H).

후처리

  1. customTo a 100 mL RB flask fitted with magnetic stirrer
  2. extractionextracted with ethyl acetate (50 mL)
  3. washThe organic layer was washed with sodium thiosulphate solution (30 mL), water (30 mL) and saturated brine solution (10 mL)
  4. dry with materialThe organic layer was dried over anhydrous Na2SO4
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-fda15d37112f4d62a8fe5323a8e6e953
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278915B2

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