Water → methyl 6-chloro-3,4-dihydro-2,4-dimethyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate

HRID 329712노트

반응식

HRID 329712 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:14]([O:16][CH3:17])=[O:15])[C:5]2[O:10][CH:9]([CH3:11])[C:8](=[O:12])[NH:7][C:6]=2[CH:13]=1.[CH3:18]C(C)([O-])C.[K+].CI.O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]([C:14]([O:16][CH3:17])=[O:15])[C:5]2[O:10][CH:9]([CH3:11])[C:8](=[O:12])[N:7]([CH3:18])[C:6]=2[CH:13]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 14517232methyl 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 14517233methyl 6-chloro-3,4-dihydro-2,4-dimethyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate수율 99.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of 4.85 g of methyl 6-chloro-3,4-dihydro-2-methyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate in 30 ml of dimethylformamide is added 2.7 g of potassium t-butoxide and solution stirred at room temperature for 30 minutes. To the resultant solution is added dropwise a solution of 3.4 g of methyl iodide in 10 ml of dimethylformamide under stirring. After the reaction solution is stirred for 1.5 hours, 200 ml of water is added thereto. The insoluble substance is collected by filtration, washed with water and dried to give 5.1 g of methyl 6-chloro-3,4-dihydro-2,4-dimethyl-3-oxo-2H-1,4-benzoxazine-8-carboxylate, melting at 128°-130° C.

후처리

  1. stirringunder stirring
  2. stirringAfter the reaction solution is stirred for 1.5 hours
  3. filtrationThe insoluble substance is collected by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-ac25233644c04faf8123f0fef24e646d
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892872

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