Sodium hydride → 3-[4-[14-(Trimethylsilyl)tetradecylamino]benzoyl]-2,4-pentanedione

HRID 652040

반응식

HRID 652040 반응식
[CH3:1][C:2](=[O:7])[CH2:3][C:4](=[O:6])[CH3:5].[H-].[Na+].Cl.[CH3:11][Si:12]([CH3:38])([CH3:37])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][NH:27][C:28]1[CH:36]=[CH:35][C:31]([C:32](Cl)=[O:33])=[CH:30][CH:29]=1>COCCOC>[CH3:11][Si:12]([CH3:38])([CH3:37])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][NH:27][C:28]1[CH:36]=[CH:35][C:31]([C:32]([CH:3]([C:2](=[O:7])[CH3:1])[C:4](=[O:6])[CH3:5])=[O:33])=[CH:30][CH:29]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 31261AcetylacetoneHCID 201982304-[14-(Trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride

생성물 1

HCID 201982483-[4-[14-(Trimethylsilyl)tetradecylamino]benzoyl]-2,4-pentanedione

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매3회

실험 절차

A solution of 14.2 g. of 2,4-pentanedione and 20 ml. of 1,2-dimethoxyethane is added to a suspension of 6.8 g. of sodium hydride in 110 ml. of 1,2-dimethoxyethane under argon. A solution of 14.0 g. of 4-[14-(trimethylsilyl)tetradecylamino]benzoyl chloride hydrochloride in 1,2-dimethoxyethane is then added. The reaction mixture is stirred at room temperature for 12 hours, cooled, poured on ice and extracted with ether. The ether solution is washed with water and saturated sodium chloride solution, dried with anhydrous sodium sulfate and evaporated. The residue is then chromatographed over silica gel to yield the product as a white solid.

후처리

  1. temperaturecooled
  2. additionpoured on ice
  3. extractionextracted with ether
  4. washThe ether solution is washed with water and saturated sodium chloride solution
  5. dry with materialdried with anhydrous sodium sulfate
  6. customevaporated
  7. customThe residue is then chromatographed over silica gel

출처 및 근거

ORD 기록
ord-e024bcba5a4c4df882da6a6d92b9da44
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04670421

연결된 노트

불러오는 중…