Hydrochloric Acid → 3,4-Dihydro-2-methyl-4-oxo-2H-1,2-benzothiazine-3-carboxylic Acid-1,1-dioxide

HRID 2119205노트

반응식

HRID 2119205 반응식
[CH3:1][N:2]1[CH2:7][C:6](=[O:8])[C:5]2[CH:9]=[CH:10][CH:11]=[CH:12][C:4]=2[S:3]1(=[O:14])=[O:13].[C:15](=O)([O-:17])[O-:16].C[Mg+2].Cl.C(OCC)C>CN(C)C=O>[CH3:1][N:2]1[CH:7]([C:15]([OH:17])=[O:16])[C:6](=[O:8])[C:5]2[CH:9]=[CH:10][CH:11]=[CH:12][C:4]=2[S:3]1(=[O:13])=[O:14]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 76017542-methyl-2,3-dihydro-4H-1,2-benzothiazin-4-one 1,1-dioxideHCID 178526095HCID 178526095, 화합물

생성물 1

HCID 130512493,4-Dihydro-2-methyl-4-oxo-2H-1,2-benzothiazine-3-carboxylic Acid-1,1-dioxide수율 94.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 6.34 g (0.03 mole) 3,4-dihydro-2-methyl-4-oxo-1,2-benzothiazine 1,1-dioxide, 19.5 g (0.15 mole) methylmagnesiumcarbonate in 150 ml N,N-dimethyl formamide were added. The mixture was stirred at 140°-150° C. for 2 hours. The resulting solution was poured quickly into a mixture of 200 ml conc-hydrochloric acid, 200 g ice chips and 500 ml diethyl ether. After stirring the mixture for 10 minutes, the diethylether layer was separated and the separated diethyl ether solution was evaporated in vacuo. The precipitated pale yellow crystals were filtered and recrystallized in dilute methanol solution to obtain 7.21 g of the title compound as white crystals. Yield: 94%

후처리

  1. stirringAfter stirring the mixture for 10 minutes
  2. customthe diethylether layer was separated
  3. customthe separated diethyl ether solution was evaporated in vacuo
  4. filtrationThe precipitated pale yellow crystals were filtered
  5. customrecrystallized in dilute methanol solution

출처 및 근거

ORD 기록
ord-bebfab3267b043beb133eb149e204ab8
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04683306

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