4-tert-Butylbenzyl alcohol → HCID 76853235、化合物

HRID 339929

反応式

HRID 339929 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 76853235HCID 76853235、化合物収率 77%

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-93733c3d90984d0eb0ecac29f21d3b54
出典データセット
uspto-grants-2014_11
特許番号
US08895574B2

関連ノート

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