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Ammonia → 6-Bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide

HRID 638362
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HRID 638362 반응식
[Br:1][C:2]1[CH:3]=[C:4]([S:15](Cl)(=[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.[NH3:19]>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]([S:15]([NH2:19])(=[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
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4

반응물 2

HCID 222AmmoniaHCID 135920726-Bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonyl chloride

생성물 1

HCID 135920736-Bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
20 °C

실험 절차

A solution of 180 g of 6-bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonyl chloride in 500 ml of tetrahydrofuran is added dropwise over 30 minutes to 307 ml of a 30% aqueous solution of ammonia. The mixture is stirred for 30 minutes at 20° C. and concentrated under reduced pressure at 45° C. The residue is triturated with 200 ml of ether. The precipitate is isolated, washed with water and dried at 45° C., affording 63.2 g of 6-bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide of m.p. 243°-245° C. (recrystallisation from ethanol).

후처리

  1. concentrationconcentrated under reduced pressure at 45° C
  2. customThe residue is triturated with 200 ml of ether
  3. customThe precipitate is isolated
  4. washwashed with water
  5. customdried at 45° C.
  6. customaffording
  7. custom63.2 g of 6-bromo-2,2-dioxo-3-methyl-1,2-benzoxathiin-8-ylsulfonamide of m.p. 243°-245° C. (recrystallisation from ethanol)

출처 및 근거

ORD 기록
ord-6d27e9e3cad84a69b3eec0fa8ccc4448
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04560771

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