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

HRID 1282284
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HRID 1282284 반응식
[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
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참가 물질

5

반응물 2

HCID 222Ammonia2회HCID 184240653-(Chloromethyl)-2-methoxypyridine hydrochloride

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
35 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5b80d313a9df400a94f473902a13af99
출처 데이터셋
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06455671B1

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