Thionyl Chloride → 4-(tert-Butyl)-2-(chloromethyl)pyridine

HRID 963491ノート

反応式

HRID 963491 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11]O)[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].S(Cl)([Cl:15])=O>C(Cl)(Cl)Cl>[C:1]([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH2:11][Cl:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 18799645(4-(tert-Butyl)pyridin-2-yl)methanol

生成物 1

HCID 190813024-(tert-Butyl)-2-(chloromethyl)pyridine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

反応条件

温度
50 °C

実験手順

To a solution of 4-tert-butyl-2-hydroxymethylpyridine (0.36 g) in chloroform (10 ml) was added dropwise a solution of thionyl chloride (1 ml) in chloroform (5 ml) at room temperature and the mixture was stirred for 3 hours at ca. 50° C., After cooling to room temperature, the resultant mixture was concentrated in vacuo. The residue was taken up with chloroform and washed with saturated sodium carbonate aqueous solution, dried over magnesium sulfate, filtered and concentrated in vacuo to give 4-tert-butyl-2-chloromethylpyridine (0.37 g) as a brown oil.

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationthe resultant mixture was concentrated in vacuo
  3. washwashed with saturated sodium carbonate aqueous solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2a8966bd26994a7598edcf4c7e6a2a0c
出典データセット
uspto-grants-1998_06
特許番号
US05763437

反応ノート

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