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

HRID 378785ノート

反応式

HRID 378785 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 134540383,4,6-Trichloro-2-pyridinecarboxylic acid収率 93.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1b38e812deca4b08b94017f78a7e5129
出典データセット
uspto-grants-2001_10
特許番号
US06297197B1

反応ノート

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