Water → HCID 59153388, 화합물

HRID 2064753노트

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HRID 2064753 반응식
[C:1]([O-])([O-])=O.[K+].[K+].[CH3:7][O:8][C:9]([C:11]1[C:20]2[O:19][CH2:18][CH2:17][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][CH2:17][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 16244454HCID 16244454, 화합물

생성물 1

HCID 59153388HCID 59153388, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
75 °C

실험 절차

K2CO3 (4.76 mmol) is added to a solution of 3,4-dihydro-2H-benzo[1,4]oxazine-8-carboxylic acid methyl ester (2.07 mmol) in DMF (3.0 mL). After 30 min methyl iodide (4.14 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=0.83 min; [M+H]+=208.1.

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-0faa9338377c45bf9ad97952e866e195
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288435B2

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