Thionyl Chloride → 4,6-Dichloropyrimidine-5-carbonitrile

HRID 1616057

反応式

HRID 1616057 の反応式
[Cl:1][C:2]1[C:7]([CH:8]=[N:9]O)=[C:6]([Cl:11])[N:5]=[CH:4][N:3]=1.O=S(Cl)Cl>C(Cl)(Cl)Cl>[Cl:1][C:2]1[C:7]([C:8]#[N:9])=[C:6]([Cl:11])[N:5]=[CH:4][N:3]=1

参加物

4

実験手順

4,6-Dichloro-5-pyrimidinecarbaldehyde oxime (8 g) was dissolved in CHCl3 (40 mL) and treated with SOCl2 (6 mL) for 2 h at rt. The solvent was removed and the residue was dissolved in DCM (5 mL). The resulting solid was filtered and washed with DCM (5 mL). The filtrate was concentrated under reduced pressure and purified by silica gel column chromatography using DCM-hexane (3:1) to give 4,6-dichloro-5-pyrimidinecarbonitrile as a white solid.

後処理

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in DCM (5 mL)
  3. filtrationThe resulting solid was filtered
  4. washwashed with DCM (5 mL)
  5. concentrationThe filtrate was concentrated under reduced pressure
  6. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-5ec6df45510648cf809b546909897e57
出典データセット
uspto-grants-2014_07
特許番号
US08765768B2

関連ノート

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