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Potassium Carbonate → HCID 58603139, 화합물

HRID 1354220
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HRID 1354220 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[C:6]2[CH:13]1[CH2:15][O:14]1.[C:16]([O:20][C:21]([CH:23]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25][NH:24]1)=[O:22])([CH3:19])([CH3:18])[CH3:17].Cl([O-])(=O)(=O)=O.[Li+].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O.C(OCC)(=O)C>[C:16]([O:20][C:21]([CH:23]1[CH2:29][CH2:28][N:27]([CH2:15][CH:13]([OH:14])[C:6]2[C:5]3[C:10](=[CH:11][CH:12]=[C:3]([O:2][CH3:1])[CH:4]=3)[N:9]=[CH:8][CH:7]=2)[CH2:26][CH2:25][NH:24]1)=[O:22])([CH3:19])([CH3:17])[CH3:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 11298596HCID 11298596, 화합물HCID 15140404tert-Butyl 1,4-diazepane-5-carboxylateHCID 23665649Lithium perchlorate

생성물 1

HCID 58603139HCID 58603139, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

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온도
100 °C

실험 절차

A mixture of 6-methoxy-4-oxiranylquinoline (400 mg, 2 mmol), [1,4]-diazepane-5-carboxylic acid tert-butyl ester (400 mg, 2 mmol, prepared as described in J. Chem. Research (S), 1991, 306, 2876), lithium perchlorate (211 mg, 2 mmol) and potassium carbonate (275 mg, 2 mmol) in DMF (5 ml) was heated at 100° C. for 4 hours. The reaction mixture was diluted with water and ethyl acetate, the aqueous phase was extracted with ethyl acetate and the combined organic phases were dried over sodium sulphate and concentrated. The product was purified by chromatography on silica gel (DCM/MeOH 9:1).

후처리

  1. extractionthe aqueous phase was extracted with ethyl acetate
  2. dry with materialthe combined organic phases were dried over sodium sulphate
  3. concentrationconcentrated
  4. customThe product was purified by chromatography on silica gel (DCM/MeOH 9:1)

출처 및 근거

ORD 기록
ord-0102c04fe1ec4a15b95adfa8a499e9a1
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223776B2

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