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

HRID 2119205ノート

反応式

HRID 2119205 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%

後処理

  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

出典と根拠

ORDレコード
ord-bebfab3267b043beb133eb149e204ab8
出典データセット
uspto-grants-1987_07
特許番号
US04683306

反応ノート

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