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Hydrochloric Acid → 4-t-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-2-morpholino-4-pyrimidinyl]benzenesulfonamide

HRID 1418330
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HRID 1418330 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[O:28][CH3:29])=[C:19]([Cl:30])[N:18]=[C:17](Cl)[N:16]=2)(=[O:13])=[O:12])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[NH:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1.O.Cl>CS(C)=O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([S:11]([NH:14][C:15]2[C:20]([O:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=3[O:28][CH3:29])=[C:19]([Cl:30])[N:18]=[C:17]([N:32]3[CH2:37][CH2:36][O:35][CH2:34][CH2:33]3)[N:16]=2)(=[O:13])=[O:12])=[CH:9][CH:10]=1)([CH3:2])([CH3:4])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8083MorpholineHCID 867538724-t-butyl-N-[2,6-dichloro-5-(2-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide

생성물 1

HCID 227294144-t-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-2-morpholino-4-pyrimidinyl]benzenesulfonamide수율 45%

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

실험 절차

4-t-Butyl-N-[2,6-dichloro-5-(2-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide (5) (482 mg; 1.0 mmol) was dissolved in dimethyl sulfoxide (5 ml). Morpholine (175 mg; 2.0 mmol) was added to the solution, and the resultant mixture was stirred overnight at 100° C. After being cooled, the reaction mixture was poured into water, made acidic with hydrochloric acid, and extracted with ethyl acetate, being washed with water, dried over anhydrous sodium sulfate, and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2), to thereby obtain 240 mg (yield: 45%) of the title compound as a white powder.

후처리

  1. temperatureAfter being cooled
  2. extractionextracted with ethyl acetate
  3. washbeing washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=1:2)

출처 및 근거

ORD 기록
ord-ebe58f8e95514036b06e3790f3aab0ec
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05883092

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