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Carbon Dioxide → 4-Ethoxy-3-hydroxypyridine-2-carboxylic acid

HRID 1797022
ノート
印刷プレビュー

反応式

HRID 1797022 の反応式
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[O:10]COCC[Si](C)(C)C)[CH3:2].[Li]C(C)(C)C.[C:24](=[O:26])=[O:25]>C1COCC1.CCOCC>[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][N:7]=[C:6]([C:24]([OH:26])=[O:25])[C:5]=1[OH:10])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 280Carbon DioxideHCID 22175090HCID 22175090、化合物HCID 178418306HCID 178418306、化合物

生成物 1

HCID 221751134-Ethoxy-3-hydroxypyridine-2-carboxylic acid

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A stirred solution of 11 (2.9 g) in THF (50 mL) under an argon atmosphere was cooled to ≦−70° C. To this was slowly added t-BuLi (8 mL, 1.5M pentane solution) while keeping the reaction temperature at ≦−66° C. After the addition was complete, the mixture was stirred at ≦−70° C. for 45 minutes and then poured into a slurry of crushed dry ice in ether. The resulting mixture was stirred until it reached room temperature, then the solvents were evaporated. THF (25 mL) and 4N HCl (15 mL) were added to the residue and the resulting mixture was stirred at room temperature for two hours. At the end of this period, the insoluble material was filtered, washed with a small volume of THF and air dried to give the title compound as a white solid (1.05 g). Preparation of 6-Bromo-3-Benzyloxy-4-Methoxypyridine-2-Carboxylic Acid (16) and its Acid Chloride (3) (See Scheme 4). a. Preparation of Methyl 4,6-Dibromo-3-Hydroxypyridine-2-Carboxylate (14).

後処理

  1. customat ≦−66° C
  2. additionAfter the addition
  3. stirringThe resulting mixture was stirred until it
  4. customreached room temperature
  5. customthe solvents were evaporated
  6. additionTHF (25 mL) and 4N HCl (15 mL) were added to the residue
  7. stirringthe resulting mixture was stirred at room temperature for two hours
  8. filtrationAt the end of this period, the insoluble material was filtered
  9. washwashed with a small volume of THF and air
  10. customdried

出典と根拠

ORDレコード
ord-7861148a689b437c854b3aecadcae102
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07034035B2

反応ノート

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