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

HRID 2206724

反応式

HRID 2206724 の反応式
[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

参加物

3

反応物 2

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

生成物 1

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

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-22a188a88eb0429798d0ffe0eec7b1e9
出典データセット
uspto-grants-2016_06
特許番号
US09371303B2

関連ノート

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