Cesium carbonate → HCID 67131202, 화합물

HRID 1890441노트

반응식

HRID 1890441 반응식
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]=[CH:8][C:9](=[O:13])[NH:10]2)=[CH:5][CH:4]=1.[C:14]([O:18][C:19]([N:21]1[CH2:27][CH2:26][C:23]2([O:25][CH2:24]2)[CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15].C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[C:14]([O:18][C:19]([N:21]1[CH2:27][CH2:26][C:23]([OH:25])([CH2:24][N:10]2[C:11]3[C:6](=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[CH:12]=3)[CH:7]=[CH:8][C:9]2=[O:13])[CH2:22]1)=[O:20])([CH3:17])([CH3:15])[CH3:16]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 299427567-Methoxy-1,2-dihydroquinolin-2-oneHCID 42609244tert-Butyl 1-oxa-5-azaspiro[2.4]heptane-5-carboxylate

생성물 1

HCID 67131202HCID 67131202, 화합물수율 47%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

A solution of 7-methoxy-1H-quinolin-2-one (650 mg, 3.7 mmol) and 1-oxa-5-aza-spiro[2.4]heptane-5-carboxylic acid tert-butyl ester (1 eq., commercial) in DMF (10 mL) was treated with Cs2CO3 (1 eq.) and heated at 70° C. overnight. The mixture was partitioned between EA and water, the org. phase washed with water and brine, dried over MgSO4 and concentrated. The product was purified by CC (EA/Hept 1:1, EA) to give the desired intermediate as a yellowish oil (650 mg, 47% yield).

후처리

  1. customThe mixture was partitioned between EA and water
  2. washphase washed with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe product was purified by CC (EA/Hept 1:1, EA)

출처 및 근거

ORD 기록
ord-7578d55693fe4659bda49ccbec822be3
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507478B2

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