Water → 2-Ethyl-4,7-benzoxazoledione

HRID 1727240노트

반응식

HRID 1727240 반응식
FC(F)(F)C(OI(C1C=CC=CC=1)OC(=O)C(F)(F)F)=[O:4].[CH2:22]([C:24]1[O:25][C:26]2[C:27](=[C:29](N)[CH:30]=[CH:31][CH:32]=2)[N:28]=1)[CH3:23].[OH2:34]>C(#N)C.C(#N)C.O.C(OC(C)C)(C)C>[CH2:22]([C:24]1[O:34][C:29]2[C:30](=[O:4])[CH:31]=[CH:32][C:26](=[O:25])[C:27]=2[N:28]=1)[CH3:23]

참가 물질

7

반응물 3

HCID 962Water2회HCID 102317Bis(trifluoroacetoxy)iodobenzeneHCID 120715892-Ethyl-1,3-benzoxazol-4-amine

생성물 1

HCID 120715902-Ethyl-4,7-benzoxazoledione

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 7914Diisopropyl Ether용매HCID 18373917Acetonitrile--water (1/1)용매

반응 조건

온도
-5 °C

실험 절차

A solution of [bis(trifluoroacetoxy)iodo]benzene (2.2 eq.) in a mixture of acetonitrile and water (80/20) is added dropwise to a solution of 2-ethyl-1,3-benzoxazol-4-amine (1 eq.) in the same acetonitrile/water mixture maintained at −5° C. The reaction medium is then diluted with water followed by extracting with dichloromethane. The resulting organic phase is washed with water, followed by drying over sodium sulphate and concentrating in order to produce a brown paste. Purification by medium pressure chromatography on silica gel produces, after taking up in diisopropyl ether, a yellow crystalline solid. Melting point: 99° C.

후처리

  1. extractionby extracting with dichloromethane
  2. washThe resulting organic phase is washed with water
  3. dry with materialby drying over sodium sulphate
  4. concentrationconcentrating in order
  5. customto produce a brown paste
  6. customPurification by medium pressure chromatography on silica gel
  7. customproduces

출처 및 근거

ORD 기록
ord-ecd578abf75749c6a5e3b351c760ec2e
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07495021B2

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