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Methylamine → HCID 11024311, 화합물

HRID 1603558
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HRID 1603558 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.[CH3:19][NH2:20]>O1CCOCC1.C(O)C>[NH2:17][C:14]1[CH:15]=[CH:16][C:11]([S:8]([C:6]2[CH:5]=[C:4]([Br:18])[N:3]=[C:2]([NH:20][CH3:19])[CH:7]=2)(=[O:10])=[O:9])=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 110146744-[(2,6-Dibromo-4-pyridinyl)sulfonyl]aniline

생성물 1

HCID 11024311HCID 11024311, 화합물수율 69%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 312751,4-Dioxane용매

실험 절차

1.45 g (0.0037 mol) of 4-(2,6-dibromopyridine-4-sulphonyl)-phenylamine were dissolved in 40 ml of dioxane and treated with 9.6 ml of 8M methylamine in ethanol. The mixture was stirred at room temperature for 48 hrs., the solvents were removed and the residue was chromatographed on silica gel with ethyl acetate/hexane 1:3 and 1:2. The product-containing fractions, after concentration, were suspended in 50 ml of diethyl ether, treated in an ultrasound bath for 1 hr., then treated with 75 ml of hexane and the precipitate which thereby resulted was filtered off under suction. After drying in a high vacuum there was obtained 0.87 g (69%) of [4-(4-aminobenzenesulphonyl)-6-bromopyridin-2-yl]-methylamine as pale beige crystals; m.p.: 171-173° C.

후처리

  1. custom, the solvents were removed
  2. customthe residue was chromatographed on silica gel with ethyl acetate/hexane 1:3 and 1:2
  3. concentrationThe product-containing fractions, after concentration
  4. additiontreated in an ultrasound bath for 1 hr
  5. addition, then treated with 75 ml of hexane
  6. customthe precipitate which thereby resulted
  7. filtrationwas filtered off under suction
  8. customAfter drying in a high vacuum there

출처 및 근거

ORD 기록
ord-af8a4e2a506640f6832dc4d231b0334c
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05990105

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