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Diethyl Oxalate → HCID 86709894, 화합물

HRID 929483
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인쇄 미리보기

반응식

HRID 929483 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9](=[O:17])[CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C([O:20][C:21](=O)[C:22](OCC)=[O:23])C.CC(C)([O-])C.[K+]>O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N:8]1[C:9](=[O:17])[C:10]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[C:22]([OH:23])[C:21]1=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7268Diethyl OxalateHCID 364845N-(2-Chlorophenyl)-2-phenylacetamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 86709894HCID 86709894, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

After the addition of anhydride THF (20 ml) to compound 5b (1.40 g, 7.34 mmol), the temperature was adjusted to 0° C. Diethyloxalate (1.45 g, 9.50 mmol) and potassium t-butoxide (1.35 g, 11.9 mmol) were added thereto and the agitation for 3 hours was carried out. After the identification of the reaction progress with TLC, the solution was poured into the distilled water and acidified with 1N HCL aqueous solution. Three times extractions were carried out with EA and three times washings were carried out with brine. Water was removed by using Na2SO4, solvents were removed and then, crude purification was carried out by the column chromatography (EA/HX, ⅕).

후처리

  1. customwas adjusted to 0° C
  2. extractionThree times extractions
  3. customWater was removed
  4. customwere removed
  5. customcrude purification

출처 및 근거

ORD 기록
ord-f51ae69204c24faeaa80f428f5bee4af
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296690B2

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