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Morpholine → HCID 19605509, 화합물

HRID 1603588
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HRID 1603588 반응식
Br[C:2]1[CH:7]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:5]=[C:4]([Br:18])[N:3]=1.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.C(N(CC)CC)C>O1CCOCC1>[Br:18][C:4]1[CH:5]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 110146744-[(2,6-Dibromo-4-pyridinyl)sulfonyl]aniline

생성물 1

HCID 19605509HCID 19605509, 화합물수율 35.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
40 °C

실험 절차

0.211 g (0.0005 mol) of 4-(2,6-dibromopyridine-4-sulphonyl)-phenylamine was dissolved in 10 ml of dioxane and treated with 0.217 g (0.0025 mol) of morpholine and 1 ml of triethylamine. The mixture was stirred at 40° C for 72 hrs. and the solvent was then removed. The residue was partitioned in ethyl acetate and water and the organic phase was extracted with sat. sodium chloride solution and dried over MgSO4. After removal of the solvent the residue was chromatographed on silica gel with ethyl acetate/hexane 1:1 and there was obtained 0.07 g (35%) of 4(2-bromo-6-morpholine-4-ylpyridine-4-sulphonyl)-phenylamine as white crystals; m.p.: 244-245° C.

후처리

  1. customand the solvent was then removed
  2. customThe residue was partitioned in ethyl acetate
  3. extractionwater and the organic phase was extracted with sat. sodium chloride solution
  4. dry with materialdried over MgSO4
  5. customAfter removal of the solvent the residue
  6. customwas chromatographed on silica gel with ethyl acetate/hexane 1:1

출처 및 근거

ORD 기록
ord-fc9623b1b9684df0958f3a4728e4a4ba
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05990105

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