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Triethylamine → 3-Methyl-8-sulfamoyl-2,2-dioxo-1,2-benzoxathiine

HRID 638364
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HRID 638364 반응식
Br[C:2]1[CH:3]=[C:4]([S:15]([NH2:18])(=[O:17])=[O:16])[C:5]2[O:10][S:9](=[O:12])(=[O:11])[C:8]([CH3:13])=[CH:7][C:6]=2[CH:14]=1.[H][H].C(N(CC)CC)C>O1CCCC1>[O:12]=[S:9]1(=[O:11])[C:8]([CH3:13])=[CH:7][C:6]2[CH:14]=[CH:2][CH:3]=[C:4]([S:15]([NH2:18])(=[O:16])=[O:17])[C:5]=2[O:10]1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 135920736-Bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 135920743-Methyl-8-sulfamoyl-2,2-dioxo-1,2-benzoxathiine수율 75.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

120 g of 6-bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide are dissolved in 2.4 liters of tetrahydrofuran and the solution is hydrogenated with hydrogen for 40 minutes, in the presence of 41.3 g of triethylamine and 12.0 g of 5% on carbon catalyst, under normal pressure and in the temperature range from 20° to 25° C. The mixture is filtered, the filtrate is concentrated, and the residue is taken up in 1300 ml of hot 90% aqueous ethanol. The insoluble constituents are separated and the solution is cooled to 0° C. The precipitate is separated and dried, affording 70 g of 2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide of m.p. 204°-205° C.

후처리

  1. filtrationThe mixture is filtered
  2. concentrationthe filtrate is concentrated
  3. customThe insoluble constituents are separated
  4. customThe precipitate is separated
  5. customdried

출처 및 근거

ORD 기록
ord-80681d165bff4bd6b7bc83bc43a835be
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04560771

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