Ethylene Glycol → 7-Bromo-4-chloro-2-methyl-2,3-dihydrobenzofuran-5-carbonitrile

HRID 576351

반응식

HRID 576351 반응식
[CH2:1]([O:4][C:5]1[C:12]([Br:13])=[CH:11][C:8]([C:9]#[N:10])=[C:7]([Cl:14])[CH:6]=1)[CH:2]=C.[CH2:15](O)CO>>[Br:13][C:12]1[C:5]2[O:4][CH:1]([CH3:2])[CH2:15][C:6]=2[C:7]([Cl:14])=[C:8]([C:9]#[N:10])[CH:11]=1

참가 물질

3

반응물 2

HCID 174Ethylene GlycolHCID 867140364-(Allyloxy)-5-bromo-2-chlorobenzonitrile

생성물 1

HCID 710769037-Bromo-4-chloro-2-methyl-2,3-dihydrobenzofuran-5-carbonitrile수율 52%

실험 절차

The compound 38 (2.03 g, 7.45 mmol) in ethylene glycol (5 mL) was subjected to microwave conditions (Biotage®) at 250° C. for 90 min. The reaction mixture was cooled to r.t. and extracted with EtOAc/H2O (50 mL/100 mL). The organic layer was dried over MgSO4, filtered off, and evaporated in vacuo. The residue was purified using normal phase column chromatography to obtain the title product (1.05 g, 52%).

후처리

  1. extractionextracted with EtOAc/H2O (50 mL/100 mL)
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered off
  4. customevaporated in vacuo
  5. customThe residue was purified

출처 및 근거

ORD 기록
ord-5c89b694a2994ad3bbb9f04445f8f366
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09034921B2

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