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Water → 2,4-Dibromo-6-(difluoromethanesulfonyl)aniline

HRID 1995458
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HRID 1995458 반응식
[NH2:1][C:2]1[C:7]([Br:8])=[CH:6][C:5]([Br:9])=[CH:4][C:3]=1[S:10]([OH:12])=[O:11].O.Cl[CH:15]([F:17])[F:16]>C(O)(C)C.[OH-].[Na+]>[Br:8][C:7]1[CH:6]=[C:5]([Br:9])[CH:4]=[C:3]([S:10]([CH:15]([F:17])[F:16])(=[O:12])=[O:11])[C:2]=1[NH2:1]
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참가 물질

6

반응물 3

HCID 962Water2회HCID 6372ChlorodifluoromethaneHCID 13218906HCID 13218906, 화합물

생성물 1

HCID 132189132,4-Dibromo-6-(difluoromethanesulfonyl)aniline

시약·촉매·용매 2

HCID 3776Isopropanol용매HCID 14798Sodium Hydroxide용매

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온도
40 °C

실험 절차

A solution of 2-amino-3,5-dibromobenzenesulfinic acid (7.98 g; 0.025 mol) in a mixture of isopropyl alcohol (100 ml) and sodium hydroxide (8.0 g of 50% aqueous) and water (2 ml) is warmed to 40° C. Chlorodifluoromethane is added slowly through a gas inlet tube over a period of 3 hours. The reaction mixture exotherms to 55° C. The reaction mixture is poured into water (500 ml) and the solution is extracted with methylene chloride (2×100 ml). The combined extracts are washed with saturated NaHCO3 (100 ml), saturated NaCl (100 ml), then dried over MgSO4. The solvent is evaporated under vacuum yield 0.9 g of the title product, m.p. 84°-88° C.

후처리

  1. customexotherms to 55° C
  2. extractionthe solution is extracted with methylene chloride (2×100 ml)
  3. washThe combined extracts are washed with saturated NaHCO3 (100 ml), saturated NaCl (100 ml)
  4. dry with materialdried over MgSO4
  5. customThe solvent is evaporated under vacuum yield 0.9 g of the title product, m.p. 84°-88° C.

출처 및 근거

ORD 기록
ord-184d3148618a41c094bdef81d50d731c
출처 데이터셋
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04404402

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