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

HRID 473409

反応式

HRID 473409 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-2b9a09bac4be41d5a9ac0c90a8a45de4
出典データセット
uspto-grants-2014_01
特許番号
US08633313B2

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