Formaldehyde → 2-(Pyrimidin-4-yl)ethanol

HRID 854347ノート

反応式

HRID 854347 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][N:3]=1.[CH2:8]=[O:9]>CCOCC>[OH:9][CH2:8][CH2:1][C:2]1[CH:7]=[CH:6][N:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 712FormaldehydeHCID 189224-Methylpyrimidine

生成物 1

HCID 154753442-(Pyrimidin-4-yl)ethanol

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 4-methylpyrimidine (10 g, 106 mmol) and para-formaldehyde (3 g) was stirred in a 50 mL sealed capacity pressure vessel at 165° C. for 3.5 hours. After cooling, ether was added and the solvents evaporated to afford an oil. This was purified by silica column chromatography using a Flashmaster system, eluting with dichloromethane, then chloroform, ether, and finally ethyl acetate. The ethyl acetate fractions were evaporated to afford the title compound as an oil.

後処理

  1. customsealed capacity pressure vessel at 165° C. for 3.5 hours
  2. temperatureAfter cooling
  3. customthe solvents evaporated
  4. customto afford an oil
  5. customThis was purified by silica column chromatography
  6. washeluting with dichloromethane
  7. customThe ethyl acetate fractions were evaporated

出典と根拠

ORDレコード
ord-24aa06d178004867a09c8cf2f8c473d2
出典データセット
uspto-grants-2007_08
特許番号
US07259163B2

反応ノート

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