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Water → Ethyl 2,6-diisopropyl-4-(4-fluorophenyl)-5-methoxymethylpyridine-3-carboxylate

HRID 1609555
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HRID 1609555 반응식
[CH3:1]I.[H-].[Na+].[CH:5]([C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[C:11]([CH2:26][OH:27])=[C:10]([CH:28]([CH3:30])[CH3:29])[N:9]=1)([CH3:7])[CH3:6].O>O1CCCC1>[CH:5]([C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[C:12]([C:19]2[CH:20]=[CH:21][C:22]([F:25])=[CH:23][CH:24]=2)[C:11]([CH2:26][O:27][CH3:1])=[C:10]([CH:28]([CH3:29])[CH3:30])[N:9]=1)([CH3:7])[CH3:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 10291957Ethyl 2,6-Diisopropyl-4-(4-fluorophenyl)-3-hydroxymethylpyridine-5-carboxylate

생성물 1

HCID 18926957Ethyl 2,6-diisopropyl-4-(4-fluorophenyl)-5-methoxymethylpyridine-3-carboxylate

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

0.57 ml (9.2 mmol)of methyl iodide and, at -50° C., 327 mg (10.9 mmol) of 80% strength sodium hydride are added under a nitrogen atmosphere to 3 g (8.4 mmol) of the compound from Example 4 in 100 ml of dry tetrahydrofuran. The mixture is stirred for 2 hours and the temperature is allowed to rise to 25° C. in the course of this. Water is cautiously added to the mixture and it is extracted several times using ether, and the organic phase is dried over sodium sulphate and concentrated in vacuo.

후처리

  1. customto rise to 25° C. in the course
  2. extractionis extracted several times
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9f0ca6bfce40445195f839985f7c5a6e
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05401746

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