4-tert-Butylbenzyl alcohol → HCID 76853235, 화합물

HRID 339929

반응식

HRID 339929 반응식
Cl[C:2]1[C:7]([O:8][CH3:9])=[CH:6][N:5]=[CH:4][N:3]=1.[C:10]([C:14]1[CH:21]=[CH:20][C:17]([CH2:18][OH:19])=[CH:16][CH:15]=1)([CH3:13])([CH3:12])[CH3:11].[H-].[Na+]>CC(N(C)C)=O>[C:10]([C:14]1[CH:15]=[CH:16][C:17]([CH2:18][O:19][C:2]2[C:7]([O:8][CH3:9])=[CH:6][N:5]=[CH:4][N:3]=2)=[CH:20][CH:21]=1)([CH3:13])([CH3:11])[CH3:12]

참가 물질

5

반응물 3

HCID 134164-tert-Butylbenzyl alcoholHCID 24758Sodium hydrideHCID 110080394-Chloro-5-methoxypyrimidine

생성물 1

HCID 76853235HCID 76853235, 화합물수율 77%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

To a solution of 4-chloro-5-methoxypyrimidine (1.5 g, 10.3 mmol) described in Journal of the Chemical Society (1960), 4590, and 4-t-butylbenzylalcohol (2.55 g, 15.6 mmol) in dimethylacetamide (10 mL) was added sodium hydride (0.625 g, 15.6 mmol) at 0° C., and the mixture was stirred at room temperature for 3 hrs. The reaction mixture was poured into ice water, and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 4-(4-t-butylbenzyloxy)-5-methoxypyrimidine (2.16 g).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationthe solvent was concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-93733c3d90984d0eb0ecac29f21d3b54
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895574B2

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