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Hydrochloric Acid → 5-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-malononitrile

HRID 49015
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인쇄 미리보기

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HRID 49015 반응식
Cl[C:2]1[C:6]2[CH:7]=[C:8]([N:11]3[C:16](=[O:17])[CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[N:13]([CH3:22])[C:12]3=[O:23])[CH:9]=[CH:10][C:5]=2[S:4][N:3]=1.[C:24](#[N:28])[CH2:25][C:26]#[N:27].C(N(CC)CC)C.Cl>CS(C)=O.O.[Cl-].[Na+].O>[CH3:22][N:13]1[C:14]([C:18]([F:21])([F:20])[F:19])=[CH:15][C:16](=[O:17])[N:11]([C:8]2[CH:9]=[CH:10][C:5]3[S:4][N:3]=[C:2]([CH:25]([C:24]#[N:28])[C:26]#[N:27])[C:6]=3[CH:7]=2)[C:12]1=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 8010MalononitrileHCID 8471TriethylamineHCID 159065613-(3-chloro-1,2-benzisothiazol-5-yl)-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 221198185-[3,6-Dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-1,2-benzisothiazole-3-malononitrile

시약·촉매·용매 3

HCID 679
Dimethyl Sulfoxide
용매
HCID 962Water용매
HCID 57417360Sodium chloride; water용매

반응 조건

온도
60 °C

실험 절차

A mixture of 3-(3-chloro-1,2-benzisothiazol-5-yl)-1-methyl-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione (0.500 g), malononitrile (0.270 g) and triethylamine (1.50 g) in methyl sulfoxide is stirred at 60° C. for 15 minutes, cooled to room temperature, and diluted with water. The resultant aqueous mixture is extracted with ethyl acetate. The organic extract is washed with water, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain a brown oil. The extracted aqueous phase is diluted with brine, acidified with concentrated hydrochloric acid, and extracted with ethyl acetate. The organic extract is dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a brown oil. Flash column chromatography of the combined oils using silica gel and an ethyl acetate/hexanes/methanol/acetic acid solution (10:10:4:1) gives the title product as an oil which is identified by NMR spectral analyses.

후처리

  1. temperaturecooled to room temperature
  2. extractionThe resultant aqueous mixture is extracted with ethyl acetate
  3. extractionThe organic extract
  4. washis washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated in vacuo
  7. customto obtain a brown oil
  8. extractionextracted with ethyl acetate
  9. extractionThe organic extract
  10. dry with materialis dried over anhydrous magnesium sulfate
  11. concentrationconcentrated in vacuo
  12. customto obtain a brown oil

출처 및 근거

ORD 기록
ord-8cefe8f0358940d98a5f63ae39284fe8
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06706663B2

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