Potassium Carbonate → HCID 22252247, 화합물

HRID 1611963노트

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HRID 1611963 반응식
[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([NH2:12])[O:11][C:7]=2[C:6]([NH2:13])=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].I[CH2:21][CH2:22][O:23][CH2:24][CH2:25]I>CN(C=O)C>[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([NH2:12])[O:11][C:7]=2[C:6]([N:13]2[CH2:25][CH2:24][O:23][CH2:22][CH2:21]2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 34307791-Iodo-2-(2-iodoethoxy)ethaneHCID 22252238HCID 22252238, 화합물

생성물 1

HCID 22252247HCID 22252247, 화합물수율 53%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

To a stirred solution of 800 mg (4.47 mmol) 4-methoxy-benzooxazole-2,7-diamine in 40 ml DMF at room temperature were added 2.47 g (17.9 mmol) potassium carbonate and 2.18 g (6.70 mmol) 1-iodo-2-(2-iodo-ethoxy)-ethane and the mixture heated at 60° C. for 48 h. After cooling to room temperature the mixture was poured onto water and extracted three times with ethyl acetate. The combined organic phases were washed with brine, then dried over sodium sulphate and concentrated in vacuo. Flash chromatography (2/98 methanol/dichloromethane, then 10/90 methanol/dichloromethane) afforded 585 mg (53%) 4-methoxy-7-morpholin-4-yl-benzooxazol-2-ylamine as a light brown solid. ES-MS m/e (%): 250 (M+H+, 100).

후처리

  1. temperatureAfter cooling to room temperature the mixture
  2. additionwas poured onto water
  3. extractionextracted three times with ethyl acetate
  4. washThe combined organic phases were washed with brine
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-afdc7b2623844dd6b0d59e2767512259
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06992083B2

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