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

HRID 2206724

반응식

HRID 2206724 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-22a188a88eb0429798d0ffe0eec7b1e9
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09371303B2

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