Hydrochloric Acid → {[5-(1-Methyl-1-hydroxyethyl)isoxazol-3-yl]methyl}malononitrile

HRID 2261353노트

반응식

HRID 2261353 반응식
[OH:1][C:2]([C:5]1[O:9][N:8]=[C:7]([CH:10]=[C:11]([C:14]#[N:15])[C:12]#[N:13])[CH:6]=1)([CH3:4])[CH3:3].[BH4-].[Na+].Cl>O1CCCC1>[OH:1][C:2]([C:5]1[O:9][N:8]=[C:7]([CH2:10][CH:11]([C:12]#[N:13])[C:14]#[N:15])[CH:6]=1)([CH3:4])[CH3:3]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 4311764Sodium borohydrideHCID 57736335{[5-(1-Hydroxy-1-methylethyl)-isoxazol-3-yl]methylidene}malononitrile

생성물 1

HCID 57736354{[5-(1-Methyl-1-hydroxyethyl)isoxazol-3-yl]methyl}malononitrile수율 53.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

9.91 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methylidene}malononitrile was dissolved in 100 ml of tetrahydrofuran, and 3.78 g of sodium borohydride was then added under ice-cooling. The mixture was stirred for 8 hours under ice-cooling. The reaction mixture was added to 0.5 N hydrochloric acid over 30 minutes and then extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 5.38 g of {[5-(1-hydroxy-1-methylethyl)-isoxazol-3-yl]methyl}malononitrile.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c381e5a3887b48ce80b4ef37c5f71cd9
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07846956B2

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