Water → HCID 59153391, 화합물

HRID 560272노트

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HRID 560272 반응식
[C:1]([O-])([O-])=O.[K+].[K+].[CH3:7][O:8][C:9]([C:11]1[C:20]2[O:19][CH2:18][C:17](=[O:21])[NH:16][C:15]=2[CH:14]=[CH:13][CH:12]=1)=[O:10].CI.O>CN(C=O)C.CCOC(C)=O>[CH3:7][O:8][C:9]([C:11]1[C:20]2[O:19][CH2:18][C:17](=[O:21])[N:16]([CH3:1])[C:15]=2[CH:14]=[CH:13][CH:12]=1)=[O:10]

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 23770643Methyl 3-oxo-3,4-dihydro-2H-1,4-benzoxazine-8-carboxylate

생성물 1

HCID 59153391HCID 59153391, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
75 °C

실험 절차

K2CO3 (6.66 mmol) is added to a solution of 3-oxo-3,4-dihydro-2H-benzo[1,4]oxazine-8-carboxylic acid methyl ester (2.90 mmol) in DMF (10 mL). After 30 min methyl iodide (5.79 mmol) is added and the mixture is stirred for 2 h at 75° C. Cold water and EtOAc are added, the layers are separated and the aq. layer is extracted with EtOAc. The combined organic layers are washed with water and brine, dried over MgSO4 and concentrated in vacuo to give a crude product which is used without further purification. LC-MS: tR=0.76 min; [M+H]+=222.2.

후처리

  1. customthe layers are separated
  2. extractionthe aq. layer is extracted with EtOAc
  3. washThe combined organic layers are washed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-b64c639d6ec34cc3b9073ee933896b20
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063099B2

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