Water → HCID 59153391、化合物

HRID 560272ノート

反応式

HRID 560272 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

HCID 59153391HCID 59153391、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b64c639d6ec34cc3b9073ee933896b20
出典データセット
uspto-grants-2011_11
特許番号
US08063099B2

反応ノート

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