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

HRID 456596

반응식

HRID 456596 반응식
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

참가 물질

8

반응물 6

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-b2a5bce6931b4469875ced99a3d86bcb
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186730B2

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