Diethyl Oxalate → HCID 86709896, 화합물

HRID 929485노트

반응식

HRID 929485 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:17])[CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:4][CH:3]=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:3]=[CH:4][C:5]([N:8]2[C:9](=[O:17])[C:10]([C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)=[C:22]([OH:23])[C:21]2=[O:20])=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 7268Diethyl OxalateHCID 723395N-(4-chlorophenyl)-2-phenylacetamideHCID 23665647Potassium tert-butoxide

생성물 1

HCID 86709896HCID 86709896, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

After the addition of anhydride THF (20 ml) to compound 5d (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 and solvents were removed. Crude purification was carried out by the column chromatography but the next reaction was followed since the purified compound was small in quantity.

후처리

  1. customwas adjusted to 0° C
  2. extractionThree times extractions
  3. customWater was removed
  4. customwere removed
  5. customCrude purification
  6. customthe next reaction

출처 및 근거

ORD 기록
ord-9efd6477fa3749779e2689f7b7d7a725
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296690B2

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