2,6-Lutidine → 2,6-Lutidine hydrochloride

HRID 323783

반응식

HRID 323783 반응식
[N:1]1[C:6]([CH3:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8].C1(S([Cl:23])(=O)=O)C(F)=C(F)C(F)=C(F)C=1F.S(Cl)(Cl)(=O)=O>CC(C)=O.NC1C=CC=CC=1>[ClH:23].[N:1]1[C:6]([CH3:7])=[CH:5][CH:4]=[CH:3][C:2]=1[CH3:8]

참가 물질

6

반응물 3

HCID 79372,6-LutidineHCID 24648Sulfuryl chlorideHCID 700262,3,4,5,6-Pentafluorobenzenesulfonyl chloride

생성물 1

HCID 5191162,6-Lutidine hydrochloride

시약·촉매·용매 2

HCID 180Acetone용매HCID 6115Aniline용매2회

실험 절차

Aniline 9.3 (44.6 g, 268 mmol) and 2,6-lutidine (32.8 mL, 282 mmol) were dissolved in 800 mL of acetone (the aniline only partly dissolved). An addition funnel was charged with C6F5SO2Cl (41.8 mL, 282 mmol) and the sulfonyl chloride was added over 15 minutes. During the addition, the starting material dissolved and a new precipitate (2,6-lutidine hydrochloride) formed. After 30 minutes, the 2,6-lutidine hydrochloride was removed by filtration and the filtrate concentrated under reduced pressure. The brown oily solid so produced was triturated with CH2Cl2 and the solid collected. A second batch of product was obtained by repeating the concentration, trituration, and filtration. After drying under high vacuum, 95.5 g (90%) of sulfonamide 9.4 was obtained as a pale yellow solid.

후처리

  1. dissolutiononly partly dissolved)
  2. additionDuring the addition
  3. dissolutionthe starting material dissolved

출처 및 근거

ORD 기록
ord-e685f8520597489c906543d6701410b5
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06214880B1

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