Sodium hydride → HCID 178511712, 화합물

HRID 22943

반응식

HRID 22943 반응식
[H-].[Na+].Cl.[NH2:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]1.Cl[C:13]1[N:18]=[CH:17][CH:16]=[CH:15][N:14]=1>O1CCCC1>[N:14]1[CH:15]=[CH:16][CH:17]=[N:18][C:13]=1[O:11][C@H:8]1[CH2:9][CH2:10][C@H:5]([NH2:4])[CH2:6][CH2:7]1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 744042-ChloropyrimidineHCID 178479278HCID 178479278, 화합물

생성물 1

HCID 178511712HCID 178511712, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

60% sodium hydride was added to 10 ml of a tetrahydrofuran suspension containing 1.00 g of trans-4-aminocyclohexanol hydrochloride and the mixture was refluxed for 1 hour. After cooling to room temperature, 2-chloropyrimidine was slowly added thereto and the mixture was stirred at room temperature for 6 hours. The reaction mixture was poured into ice-cold water and extracted with chloroform. The extract was washed with brine and dried over anhydrous sodium sulfate, and then, the solvent was removed under reduced pressure. The residue was purified by NH-silica gel column chromatography (solvent: ethyl acetate-hexane (1:4) to chloroform alone) to obtain 788 mg of trans-4-(2-pyrimidinyloxy)cyclohexylamine (Reference Example 9-46 in Table 6).

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. additionThe reaction mixture was poured into ice-cold water
  3. extractionextracted with chloroform
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customThe residue was purified by NH-silica gel column chromatography (solvent

출처 및 근거

ORD 기록
ord-177949fd58514cb08143173f2492b15a
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849622B2

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