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

HRID 473409

반응식

HRID 473409 반응식
[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

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 760165164,6-Dichloro-5-pyrimidinecarbaldehyde oxime

생성물 1

HCID 5993714,6-Dichloropyrimidine-5-carbonitrile

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2b9a09bac4be41d5a9ac0c90a8a45de4
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633313B2

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