Sodium hydride → HCID 59341117, 화합물

HRID 14568

반응식

HRID 14568 반응식
[H-].[Na+].[CH2:3]([CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][NH:6]1)[CH3:4].[Cl:11][C:12]1[C:17]([F:18])=[C:16](Cl)[N:15]=[CH:14][N:13]=1.[Cl-].[NH4+]>O1CCCC1>[Cl:11][C:12]1[C:17]([F:18])=[C:16]([N:6]2[CH2:7][CH2:8][CH2:9][CH2:10][CH:5]2[CH2:3][CH3:4])[N:15]=[CH:14][N:13]=1

참가 물질

6

반응물 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 942052-EthylpiperidineHCID 112866754,6-Dichloro-5-fluoropyrimidine

생성물 1

HCID 59341117HCID 59341117, 화합물수율 75.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

0.07 g of sodium hydride (60% oil suspension) was suspended in 3 ml of tetrahydrofuran. 1 ml of tetrahydrofuran solution of 0.14 g of 2-ethylpiperidine was added dropwise at room temperature therein slowly, and the mixture was stirred for 10 minutes. Into the mixture was added dropwise 1 ml of tetrahydrofuran solution of 0.2 g of 4,6-dichloro-5-fluoropyrimidine at room temperature, and stirred for 4 hours. The reaction mixture was poured into a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with water, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.22 g of 4-chloro-6-(2-ethylpiperidino)-5-fluoropyrimidine.

후처리

  1. stirringstirred for 4 hours
  2. extractionthe mixture was extracted with tert-butyl methyl ether three times
  3. washThe organic layers were washed with water
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cfcbc0ba66804e69949d8072ec909492
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732448B2

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