Tetrahydrofuran → 5-(2-Hydroxy-ethyl)-3H-benzoxazol-2-one

HRID 456596

反応式

HRID 456596 の反応式
N1S[N:4]=[C:3]2[CH:6]=[C:7]([CH2:10][C:11]#N)[CH:8]=[CH:9][C:2]=12.[H-].[Al+3].[Li+].[H-].[H-].[H-].[H-].[OH-:20].[Na+].S([O-])([O-])(=O)=[O:23].[Mg+2].[O:28]1[CH2:32]CCC1>O>[OH:20][CH2:11][CH2:10][C:7]1[CH:8]=[CH:9][C:2]2[O:23][C:32](=[O:28])[NH:4][C:3]=2[CH:6]=1

参加物

8

反応物 6

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 24083Sulfuric acid magnesium salt (1:1)HCID 166653HydrideHCID 21226445Aluminium lithium hydrideHCID 695224455-Cyanomethylbenz-2,1,3-thiadiazole

生成物 1

HCID 179812295-(2-Hydroxy-ethyl)-3H-benzoxazol-2-one収率 65%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Ester (a) (0.95 g, 4.29 mmol) was added portionwise to a cold solution (0° C.) of lithium aluminium hydride (0.206 g, 4.7 mmol) in tetrahydrofuran (20 ml). The mixture was then stirred 1.5 hours at room temperature and cooled again. The excess of hydride was hydrolysed by careful addition of water (0.2 ml), 5N aqueous sodium hydroxide solution (0.2 ml) and finally water (0.6 ml). Magnesium sulfate was added and the mixture was filtered. The filtrate was concentrated to dryness to give the product (0.5 g, 65%).

後処理

  1. temperaturecooled again
  2. filtrationthe mixture was filtered
  3. concentrationThe filtrate was concentrated to dryness

出典と根拠

ORDレコード
ord-b2a5bce6931b4469875ced99a3d86bcb
出典データセット
uspto-grants-2007_03
特許番号
US07186730B2

関連ノート

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