Sodium Hydroxide → 3,4,6-Trichloro-2-pyridinecarboxylic acid

HRID 378785노트

반응식

HRID 378785 반응식
[Cl:1][C:2]1[C:3]([C:10]([O:12]C)=[O:11])=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[Cl:8].[OH-].[Na+]>CO>[Cl:1][C:2]1[C:3]([C:10]([OH:12])=[O:11])=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[Cl:8]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22677534Methyl 3,4,6-trichloropyridine-2-carboxylate

생성물 1

HCID 134540383,4,6-Trichloro-2-pyridinecarboxylic acid수율 93.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To methyl 3,4,6-Trichloropicolinate (3.57 g, 14.85 mmol) in 20 mL of methanol was added 1N NaOH (14.85 mL, 14.85 mmol). The reaction mixture was stirred at room temperature for 1 hr and then concentrated to dryness in vacuo. 100 mL each of diethyl ether and H2O were added. Aqueous layer was acidified with 1N HCl until pH=2. Methylene chloride was added and the aqueous phase was extracted with additional CH2Cl2 (2×100 mL). The combined extracts were dried (MgSO4) and concentrated to give 3.13 g of a white solid. 1H NMR(CDCl3): δ 7.50 (s, 1H).

후처리

  1. concentrationconcentrated to dryness in vacuo
  2. addition100 mL each of diethyl ether and H2O were added
  3. additionMethylene chloride was added
  4. extractionthe aqueous phase was extracted with additional CH2Cl2 (2×100 mL)
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1b38e812deca4b08b94017f78a7e5129
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06297197B1

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