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Ammonia → 1-(2-Methoxypyridin-3-yl)methanamine--hydrogen chloride (1/2)

HRID 1282284
ノート
印刷プレビュー

反応式

HRID 1282284 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[C:9]([CH2:10][Cl:11])=[CH:8][CH:7]=[CH:6][N:5]=1.[NH3:12]>O.CO>[ClH:11].[ClH:1].[CH3:2][O:3][C:4]1[C:9]([CH2:10][NH2:12])=[CH:8][CH:7]=[CH:6][N:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 222Ammonia2 回HCID 184240653-(Chloromethyl)-2-methoxypyridine hydrochloride

生成物 1

HCID 184240711-(2-Methoxypyridin-3-yl)methanamine--hydrogen chloride (1/2)

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
35 °C

実験手順

15.1 g of 2-methoxy-3-picolyl chloride hydrochloride (77.76 mmol) were slowly added dropwise to a mixture of 600 ml of 30% strength ammonia solution in water and 250 ml of methanol at 35° C. while continuously passing in gaseous ammonia. After the solution had been stirred at 35° C. for 1 h it was concentrated under reduced pressure in a rotary evaporator, the residue was made alkaline with 20% strength NaOH solution (water phases were kept small) and extracted several times with DCM, and the org. phases were dried over magnesium sulfate and concentrated under reduced pressure in a rotary evaporator. The residue was taken up in ether and, after addition of ethereal hydrochloric acid, filtration with suction and washing of the precipitate with ether, 11.0 g (67%) of 2-methoxy-3-picolylamine.2HCl were obtained as white crystals.

後処理

  1. concentrationwas concentrated under reduced pressure in a rotary evaporator
  2. extractionextracted several times with DCM
  3. dry with materialphases were dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure in a rotary evaporator
  5. additionafter addition of ethereal hydrochloric acid, filtration with suction
  6. washwashing of the precipitate with ether, 11.0 g (67%) of 2-methoxy-3-picolylamine
  7. custom2HCl were obtained as white crystals

出典と根拠

ORDレコード
ord-5b80d313a9df400a94f473902a13af99
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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