Water → 2'-[2-(1-methyl-1-phenylethyl)-2H-tetrazol-5-yl]biphenyl-4-methanol

HRID 1757496ノート

反応式

HRID 1757496 の反応式
[CH3:1][C:2]([N:10]1[N:14]=[N:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]2[CH:26]=[CH:25][C:24]([CH:27]=[O:28])=[CH:23][CH:22]=2)=[N:11]1)([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH3:3].[BH4-].[Na+].O>C(O)C>[CH3:3][C:2]([N:10]1[N:14]=[N:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]2[CH:22]=[CH:23][C:24]([CH2:27][OH:28])=[CH:25][CH:26]=2)=[N:11]1)([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1)[CH3:1]

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 15225578HCID 15225578、化合物

生成物 1

HCID 109706982'-[2-(1-methyl-1-phenylethyl)-2H-tetrazol-5-yl]biphenyl-4-methanol収率 58.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2'-[2-(1-methyl-1-phenylethyl)-2H-tetrazol-5-yl]biphenyl-4-carbaldehyde (0.62 g, 1.7 mmol), prepared as in Example 8 or 9, and sodium borohydride in 30 mL of absolute ethanol was stirred at room temperature for 1 hour. The mixture poured into 150 mL of water and the mixture was extracted withethyl acetate. The ethyl acetate layer was dried over magnesium sulfate andthen concentrated. The residue was dissolved in approximately 10 mL of absolute diethyl ether and the solution was cooled in an ice bath giving aprecipitate. The precipitate was isolated by filtration and drying gave 2'-[2-(1-methyl-1-phenylethyl)-2H-tetrazol-5-yl]biphenyl-4-methanol (0.37 g, 1.0 mmol), m.p. 119°-120° C.

後処理

  1. extractionthe mixture was extracted withethyl acetate
  2. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  3. concentrationandthen concentrated
  4. dissolutionThe residue was dissolved in approximately 10 mL of absolute diethyl ether
  5. temperaturethe solution was cooled in an ice bath
  6. customgiving aprecipitate
  7. customThe precipitate was isolated by filtration
  8. customdrying

出典と根拠

ORDレコード
ord-ca3f791365394bf99c7fd1896bac2b24
出典データセット
uspto-grants-1995_08
特許番号
US05446121

反応ノート

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