Potassium sodium tartarate → HCID 22005358、化合物

HRID 36917ノート

反応式

HRID 36917 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([CH:19]([CH3:21])[CH3:20])[N:11]=[C:10]([O:22][CH3:23])[C:9]=2[C:24](OC)=[O:25])=[CH:4][CH:3]=1.[H-].C([Al+]CC(C)C)C(C)C.C(C(C(C([O-])=O)O)O)([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([CH:19]([CH3:21])[CH3:20])[N:11]=[C:10]([O:22][CH3:23])[C:9]=2[CH2:24][OH:25])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 9855836Potassium sodium tartarateHCID 21225700DiisobutylaluminumhydrideHCID 537701363-Methyl 5-ethyl 4-(4-fluorophenyl)-6-isopropyl-2-methoxy-pyridine-3,5-dicarboxylate

生成物 1

HCID 22005358HCID 22005358、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
-78 °C

実験手順

1.48 g (3.95 mmol) of the compound from Example 5 are dissolved in 30 ml of toluene, the solution is cooled to -78° C. under nitrogen and 6.6 ml (10 mmol) of a 1.5 molar solution of diisobutylaluminium hydride in toluene are added dropwise at this temperature. The cooling bath is removed and the mixture is stirred at room temperature for 2 h. After hydrolysis using 20% strength aqueous potassium sodium tartrate solution, the organic phase is separated off, the aqueous phase is washed three times with toluene, and the combined organic phases are washed with saturated sodium chloride solution and dried using sodium sulphate.

後処理

  1. customThe cooling bath is removed
  2. customAfter hydrolysis
  3. customthe organic phase is separated off
  4. washthe aqueous phase is washed three times with toluene
  5. washthe combined organic phases are washed with saturated sodium chloride solution
  6. customdried

出典と根拠

ORDレコード
ord-0cdd43d2293f4b07afd31b99a9d6e306
出典データセット
uspto-grants-1995_05
特許番号
US05418243

反応ノート

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