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Hydrochloric Acid → 3-(Chloromethyl)-2-methoxypyridine hydrochloride

HRID 1282283
ノート
印刷プレビュー

反応式

HRID 1282283 の反応式
S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7]1[C:12]([CH2:13]O)=[CH:11][CH:10]=[CH:9][N:8]=1.[ClH:15]>C(Cl)Cl>[ClH:3].[CH3:5][O:6][C:7]1[C:12]([CH2:13][Cl:15])=[CH:11][CH:10]=[CH:9][N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 10630565(2-Methoxypyridin-3-yl)methanol

生成物 1

HCID 184240653-(Chloromethyl)-2-methoxypyridine hydrochloride収率 81%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

51 ml of thionyl chloride (696.67 mmol) were added dropwise to 17 g of 2-methoxy-3-picolyl alcohol.HCl (96.76 mmol) suspended in 60 ml of DCM, the solution was stirred at room temperature for 1 h, the solvent and excess thionyl chloride were removed under reduced pressure, and the residue was codistilled 4 times with methanol under reduced pressure and subsequently extracted by stirring with ether. 15.2 g of is 2-methoxy-3-picolyl chloride hydrochloride (81%) were obtained as a white crystalline salt.

後処理

  1. customthe solvent and excess thionyl chloride were removed under reduced pressure
  2. extractionsubsequently extracted
  3. stirringby stirring with ether

出典と根拠

ORDレコード
ord-9940ffdcdbe34c05b56d73fd6bbd2c25
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455671B1

反応ノート

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