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Thionyl Chloride → 2,6-Difluoro-4-methoxybenzonitrile

HRID 466491
ノート
印刷プレビュー

反応式

HRID 466491 の反応式
S(Cl)(Cl)=O.[F:5][C:6]1[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[C:11]([F:17])[C:7]=1[C:8]([NH2:10])=O>CN(C=O)C>[F:5][C:6]1[CH:14]=[C:13]([O:15][CH3:16])[CH:12]=[C:11]([F:17])[C:7]=1[C:8]#[N:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 27787702,6-Difluoro-4-methoxybenzamide

生成物 1

HCID 27787722,6-Difluoro-4-methoxybenzonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A solution of thionyl chloride (139.0 g, 1.17 mol) in dry DMF (150 ml) was added to a stirred solution of compound 26 (20.0 g, 0.11 mol) in dry DMF (250 ml) at room temperature. The mixture was stirred at room temperature overnight and then poured onto ice-water. The product was extracted into ether (twice), and the combined ethereal extracts were washed with water, saturated sodium hydrogen carbonate, water and dried (MgSO4). The solvent was removed in vacuo to give off-white crystals.

後処理

  1. additionpoured onto ice-water
  2. extractionThe product was extracted into ether (twice), and the combined ethereal extracts
  3. washwere washed with water, saturated sodium hydrogen carbonate, water
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed in vacuo
  6. customto give off-white crystals

出典と根拠

ORDレコード
ord-ec772511e3f64619a63fe8ef27fddd87
出典データセット
uspto-grants-1992_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05156763

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート