Potassium sodium tartarate → HCID 22005358, 화합물

HRID 36917노트

반응식

HRID 36917 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 22005358HCID 22005358, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
-78 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0cdd43d2293f4b07afd31b99a9d6e306
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05418243

반응 노트

불러오는 중…