Sodium Hydroxide → 1,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

HRID 1976272노트

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HRID 1976272 반응식
Br.Br[CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1.[OH-:22].[Na+]>O>[OH:22][CH:3]1[C:8]([C:9]2[C:14]([O:15][CH3:16])=[CH:13][C:12]([O:17][CH3:18])=[CH:11][C:10]=2[O:19][CH3:20])=[CH:7][CH2:6][N:5]([CH3:21])[CH2:4]1

참가 물질

4

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온도
20 °C

실험 절차

50 g (0.118 mol of 3(R,S)-bromo-1-methyl4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine hydrobromide (VI) were heated under reflux for 2 h in 100 ml of water. The reaction mixture was then cooled to 20° C. and adjusted to pH 12.5 by dropwise addition of 30 ml of 30% strength sodium hydroxide solution. After a short time, a pale brown precipitate crystallized out. The mixture was stirred at 5-10° C. for a further 1 h, and the precipitated product was filtered off with suction and washed with 30 ml of water. The crude product was then stirred with 20 ml of acetone, filtered off with suction and dried in vacuo.

후처리

  1. customAfter a short time, a pale brown precipitate crystallized out
  2. filtrationthe precipitated product was filtered off with suction
  3. washwashed with 30 ml of water
  4. stirringThe crude product was then stirred with 20 ml of acetone
  5. filtrationfiltered off with suction
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-f8b7f93710434a328b0039240fa46cef
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06225473B1

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