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Ammonium Chloride → HCID 22934986、化合物

HRID 916592
ノート
印刷プレビュー

反応式

HRID 916592 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1.C([Li])(C)(C)C.[C:16]([O:24][CH2:25][CH2:26][C:27]1[CH:34]=[CH:33][C:30]([CH:31]=[O:32])=[CH:29][CH:28]=1)(=[O:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[Cl-].[NH4+]>C(OCC)C>[C:16]([O:24][CH2:25][CH2:26][C:27]1[CH:28]=[CH:29][C:30]([CH:31]([C:10]2[CH:9]=[CH:8][N:7]=[CH:6][C:5]=2[O:4][CH2:3][O:2][CH3:1])[OH:32])=[CH:33][CH:34]=1)(=[O:23])[C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 37543973-(Methoxymethoxy)pyridineHCID 229349784-(2-Benzoyloxyethyl)benzaldehydeHCID 178418306HCID 178418306、化合物

生成物 1

HCID 22934986HCID 22934986、化合物収率 53.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
溶媒
2 回

実験手順

To a solution of 4-(2-benzoyloxyethyl)benzyl alcohol (1.2 g) in dichloromethane (50 mL) was added manganese dioxide (12 g), and the mixture was stirred for 23 hours at room temperature. The insoluble material was removed by filtration, and the solvent of the filtrate was removed under reduced pressure to give 4-(2-benzoyloxyethyl)benzaldehyde (0.87 g). To a solution of 3-(methoxymethyloxy)pyridine (0.20 g) in diethyl ether (20 mL) was added tert-butyllithium (1.51 mol/L solution in pentane, 1.2 mL) at −78° C., and the mixture was stirred for 30 minutes. To the reaction mixture was added a solution of 4-(2-benzoyloxy-ethyl)benzaldehyde (0.44 g) in diethyl ether (4 mL). The temperature was raised to room temperature, and the mixture was stirred for 1 hour. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous sodium sulfate, and the solvent was removed under reduced pressure. To the residue were added hexane and ethyl acetate, and the resulting crystals were collected by filtration and dried under reduced pressure to give 4-(2-benzoyloxyethyl)phenyl-3-(methoxymethyloxy)pyridin-4-yl-methanol (0.30 g). To a solution of the obtained 4-(2-benzoyloxyethyl)phenyl-3-(methoxymethyloxy)pyridin-4-yl-methanol (0.28 g) in ethanol (4.8 mL) was added concentrated hydrochloric acid (0.6 mL), and the mixture was heated under reflux for 10 minutes. The solvent of the reaction mixture was removed under reduced pressure, and ethyl acetate was added to the residue. The resulting precipitated crystals were collected by filtration and dried to give4-(2-benzoyloxyethyl)-phenyl-3-hydroxypyridin-4-ylmethanol hydrochloride (0.28 g). To a solution of the obtained 4-(2-benzoyloxyethyl)phenyl-3-hydroxypyridin-4-ylmethanol hydrochloride (0.27 g) in ethanol (6.9 mL) was added 10% palladium carbon powder (0.27 g), and the mixture was stirred for 3.5 hours at room temperature under a hydrogen atmosphere. The insoluble material was removed by filtration, and the solvent of the filtrate was removed under reduced pressure. To the residue were added ethyl acetate and diethyl ether, and the resulting crystals were collected by filtration. To the obtained crystals was added saturated aqueous sodium bicarbonate solution, and the mixture was extracted with ethyl acetate. After the organic layer was washed with brine and dried over anhydrous sodium sulfate, the solvent was removed under reduced pressure. To the residue was added diethyl ether, and the resulting precipitated crystals were collected by filtration and dried under reduced pressure to give 4-[4-(2-benzoyloxyethyl)benzyl]-3-hydroxypyridine (0.12. g).

後処理

  1. stirringthe mixture was stirred for 1 hour
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customthe solvent was removed under reduced pressure
  6. additionTo the residue were added hexane and ethyl acetate
  7. filtrationthe resulting crystals were collected by filtration
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-241b1ed7dce8480a821c58c06da53a36
出典データセット
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07271153B2

反応ノート

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