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Sodium Hydroxide → HCID 10177222, 화합물

HRID 896485
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HRID 896485 반응식
[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:27]=[CH:26][C:13]([CH2:14][CH:15]([C:21]([O:23]CC)=[O:22])[C:16]([O:18]CC)=[O:17])=[CH:12][CH:11]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1.[OH-].[Na+]>O1CCCC1>[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:11]=[CH:12][C:13]([CH2:14][CH:15]([C:16]([OH:18])=[O:17])[C:21]([OH:23])=[O:22])=[CH:26][CH:27]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 10159558Diethyl 2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}malonate

생성물 1

HCID 10177222HCID 10177222, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

Dissolve the compound obtained in Example 2 (1.5 g) in tetrahydrofuran (20 ml). Add 2N sodium hydroxide (8 ml) to the reaction mixture, cooled to 0° C. using an ice bath. Stir magnetically at ambient temperature for 72 hours. Remove the tetrahydrofuran by evaporation under reduced pressure. Take up the resulting residue in a 6N hydrochloric acid solution to pH 1 and extract twice with 50 ml of ether each time. Dry the organic phase over magnesium sulphate and remove the ether by evaporation under reduced pressure. Crystallise the resulting oil from isopropyl ether and recrystallise the resulting precipitate from cyclohexane.

후처리

  1. customRemove the tetrahydrofuran
  2. customby evaporation under reduced pressure
  3. extractionextract twice with 50 ml of ether each time
  4. dry with materialDry the organic phase over magnesium sulphate
  5. customremove the ether
  6. customby evaporation under reduced pressure
  7. customCrystallise the resulting oil from isopropyl ether
  8. customrecrystallise the resulting precipitate from cyclohexane

출처 및 근거

ORD 기록
ord-6e5ad4bd5d054d9da3036ca0da32da70
출처 데이터셋
uspto-grants-2005_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06919362B2

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