Potassium Hydroxide → 3-Benzyloxy-4-methoxypicolinic acid

HRID 350650

반응식

HRID 350650 반응식
[CH2:1]([O:8][C:9]1[C:10]([CH2:17][OH:18])=[N:11][CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[K+].[Mn]([O-])(=O)(=O)=[O:22].[K+]>O>[CH2:1]([O:8][C:9]1[C:10]([C:17]([OH:22])=[O:18])=[N:11][CH:12]=[CH:13][C:14]=1[O:15][CH3:16])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 516875Potassium PermanganateHCID 199603213-Benzyloxy-2-hydroxymethyl-4-methoxypyridine

생성물 1

HCID 199602893-Benzyloxy-4-methoxypicolinic acid수율 83.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3-Benzyloxy-2-hydroxymethyl-4-methoxypyridine (7.1 g) and 2.5 g of potassium hydroxide were suspended in 100 ml of water. While heating the suspension in a water bath, potassium permanganate (7.3 g) was added thereto, and the mixture was stirred. The precipitate was filtered, and was washed with 100 ml of methanol. The filtrate and the washings were combined, followed by concentration under the reduced pressure. The concentrate was adjusted to pH 1 by the addition of concentrated hydrochloric acid. The precipitate was filtered, washed with water, and then dried to give 6.3 g (yield 83.9%) of the title compound as colorless powder.

후처리

  1. temperatureWhile heating the suspension in a water bath
  2. filtrationThe precipitate was filtered
  3. washwas washed with 100 ml of methanol
  4. concentrationfollowed by concentration under the reduced pressure
  5. additionThe concentrate was adjusted to pH 1 by the addition of concentrated hydrochloric acid
  6. filtrationThe precipitate was filtered
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-7918c38eb2264104b46a1d5deb080734
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07183278B1

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