Dichloromethane methanol → 2,6-Dichloro-5-methoxypyrimidine-4-carbaldehyde

HRID 332921ノート

反応式

HRID 332921 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([CH:8]=C)[C:5]([O:10][CH3:11])=[C:4]([Cl:12])[N:3]=1.C[OH:14].ClCCl>>[Cl:1][C:2]1[N:7]=[C:6]([CH:8]=[O:14])[C:5]([O:10][CH3:11])=[C:4]([Cl:12])[N:3]=1

参加物

3

反応物 2

HCID 21226129Dichloromethane methanolHCID 866893262,4-Dichloro-5-methoxy-6-vinylpyrimidine

生成物 1

HCID 866893302,6-Dichloro-5-methoxypyrimidine-4-carbaldehyde

実験手順

A solution of 2,6-dichloro-5-methoxy-4-vinyl pyrimidine (6.64 g, 32.5 mmol, prepared by Example 2), in methanol:dichloromethane (1:4, 300 mL), was cooled to −78° C. in a dry ice/acetone bath. Ozone was bubbled into the reaction until the starting material was no longer present according to thin layer chromatography (TLC). Dimethyl sulfide (6 mL) was added. The mixture was concentrated on a rotary evaporator at 0° C. to remove the dichloromethane. This provided an unpurified material comprising the title compound. The title compound was not isolated from the unpurified material.

後処理

  1. customOzone was bubbled into the reaction until the starting material
  2. additionDimethyl sulfide (6 mL) was added
  3. concentrationThe mixture was concentrated on a rotary evaporator at 0° C.
  4. customto remove the dichloromethane
  5. customThis provided an unpurified material

出典と根拠

ORDレコード
ord-f1c2a354e193464487024d532308cd16
出典データセット
uspto-grants-2014_11
特許番号
US08877925B2

反応ノート

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