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Water → 2-Chloro-5-methoxybenzene-1-sulfonamide

HRID 1028396
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HRID 1028396 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[S:10](Cl)(=[O:12])=[O:11].[OH-].[NH4+:15].O>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[S:10]([NH2:15])(=[O:12])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 14923Ammonium HydroxideHCID 220335362-Chloro-5-methoxybenzene-1-sulfonyl chloride2회

생성물 1

HCID 3140422-Chloro-5-methoxybenzene-1-sulfonamide수율 95.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2-chloro-5-methoxybenzenesulfonyl chloride (2.5 g, 10.4 mmol) (i.e. the product of Step A) in tetrahydrofuran (30 mL) was added 30% ammonium hydroxide (3.0 mL, 25.7 mmol) dropwise. The reaction mixture was stirred for 15 minutes, during which time a suspension formed. To this mixture water (10 mL) was added, and the tetrahydrofuran was evaporated under reduced pressure to leave an aqueous suspension of a tan solid. The solid was isolated by filtration and washed with water to afford 2.2 g of the title compound. 1H NMR (CDCl3) δ 7.63 (d, 1H), 7.43 (d, 1H), 7.03 (d, 1H), 5.13 (br s, 2H), 3.85 (s, 3H).

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후처리

  1. customformed
  2. customthe tetrahydrofuran was evaporated under reduced pressure
  3. customto leave
  4. additionan aqueous suspension of a tan solid
  5. customThe solid was isolated by filtration
  6. washwashed with water

출처 및 근거

ORD 기록
ord-ccb2b26403a94118ac9e9a18068c8fc9
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735588B2

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