Hydrochloric Acid → HCID 86753872, 화합물

HRID 1418329

반응식

HRID 1418329 반응식
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][CH:16]=[CH:15][C:4]=1[O:5][C:6]1[C:7]([Cl:14])=[N:8][C:9]([Cl:13])=[N:10][C:11]=1Cl.[C:19]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH2:32])(=[O:31])=[O:30])=[CH:25][CH:24]=1)([CH3:22])([CH3:21])[CH3:20].[K].O.Cl>CS(C)=O>[C:19]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH:32][C:11]2[C:6]([O:5][C:4]3[CH:15]=[CH:16][CH:17]=[CH:18][C:3]=3[O:2][CH3:1])=[C:7]([Cl:14])[N:8]=[C:9]([Cl:13])[N:10]=2)(=[O:30])=[O:31])=[CH:25][CH:24]=1)([CH3:22])([CH3:20])[CH3:21]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 53746905HCID 53746905, 화합물HCID 66748434p-t-Butylbenzenesulfonamide potassium

생성물 1

HCID 86753872HCID 86753872, 화합물수율 65.1%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

5-(2-Methoxyphenoxy)-2,4,6-trichloropyrimidine (4) (4.8 g; 15.6 mmol) was dissolved in dimethyl sulfoxide (45 ml). Potassium 4-t-butylbenzenesulfonamide (8.0 g; 32 mmol) was added to the mixture while being cooled on ice, and the mixture was stirred for 30 minutes at room temperature. The reaction mixture was poured into water, made acidic with hydrochloric acid, and extracted with ethyl acetate, washed with water, dried over anhydrous sodium sulfate, and evaporated. The residue was recrystallized from ether, to thereby obtain 4.9 g (yield: 65%) of the title compound as colorless needles.

후처리

  1. temperaturewhile being cooled on ice
  2. extractionextracted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. customThe residue was recrystallized from ether

출처 및 근거

ORD 기록
ord-acd06b1c272d490387309d944c801387
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05883092

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