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Triethylamine → 1,1-dioxo-N-[4-[4-(piperidin-1-ylmethyl)pyrazol-1-yl]oxybutyl]-1,2-benzothiazol-3-amine

HRID 232026
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HRID 232026 반응식
[N:1]1([CH2:7][C:8]2[CH:9]=[N:10][N:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][NH2:18])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.Cl[C:27]1[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[S:29](=[O:37])(=[O:36])[N:28]=1>C(Cl)Cl>[N:1]1([CH2:7][C:8]2[CH:9]=[N:10][N:11]([O:13][CH2:14][CH2:15][CH2:16][CH2:17][NH:18][C:27]3[C:31]4[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=4[S:29](=[O:36])(=[O:37])[N:28]=3)[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 64783Pseudosaccharin chlorideHCID 200307904-(4-Piperidinomethylpyrazol-1-yloxy)butylamine

생성물 1

HCID 1785271931,1-dioxo-N-[4-[4-(piperidin-1-ylmethyl)pyrazol-1-yl]oxybutyl]-1,2-benzothiazol-3-amine수율 29.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

3.5 g of 4-(4-piperidinomethylpyrazol-1-yloxy)butylamine and 1.4 g of triethylamine are dissolved in 50 ml of methylene chloride. A solution of 2.8 g of 3-chlorobenzoisothiazole 1,1-dioxide in 15 ml of methylene chloride is then added dropwise. After standing for 3 hours at room temperature, the reaction mixture is washed with water, the organic phase is evaporated down and the residue is chromatographed over neutral Al2O3 (activity level III), using methylene chloride as the mobile phase. 1.7 g of the title compound are obtained, the product being crystallized from ether.

후처리

  1. washthe reaction mixture is washed with water
  2. customthe organic phase is evaporated down
  3. customthe residue is chromatographed over neutral Al2O3 (activity level III)

출처 및 근거

ORD 기록
ord-2dfd0f29ad2d434bb1dce4d38d5b1c7f
출처 데이터셋
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04851410

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