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

HRID 576351

反応式

HRID 576351 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-5c89b694a2994ad3bbb9f04445f8f366
出典データセット
uspto-grants-2015_05
特許番号
US09034921B2

関連ノート

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