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Triethylamine → HCID 67000954, 화합물

HRID 1293647
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HRID 1293647 반응식
[NH2:1][CH2:2][C:3]1[CH:8]=[C:7]([CH3:9])[N:6]=[C:5]([CH3:10])[CH:4]=1.[Br:11][C:12]1[S:16][C:15]([S:17](Cl)(=[O:19])=[O:18])=[CH:14][CH:13]=1.C(N(CC)CC)C>C1COCC1>[CH3:10][C:5]1[CH:4]=[C:3]([CH2:2][NH:1][S:17]([C:15]2[S:16][C:12]([Br:11])=[CH:13][CH:14]=2)(=[O:19])=[O:18])[CH:8]=[C:7]([CH3:9])[N:6]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27339245-Bromothiophene-2-sulfonyl chlorideHCID 135828191-(2,6-Dimethylpyridin-4-yl)methanamine

생성물 1

HCID 67000954HCID 67000954, 화합물수율 52%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred solution of commercially available 4-aminomethyl-2,6-dimethyl-pyridine [CAS-No. 324571–98–4 (0.24 g, 1.76 mmol) in THF (8 ml) was added at 0° C. (ice water bath) commercially available 5-bromo-thiophene-2-sulfonyl chloride (0.46 g, 1.76 mmol) dissolved in THF (8 ml) and triethylamine (0.27 ml, 1.94 mmol). The reaction mixture was stirred at room temperature for 16 h and evaporated. The crude product was further purified by flash chromatography (ethyl acetate/heptane) and crystallization from dichloromethane/hexane to yield the title compound (0.33 g, 52%) as a light red solid. MS (ISN) 359.0 [(M−H)−], mp 138° C.

후처리

  1. customevaporated
  2. customThe crude product was further purified by flash chromatography (ethyl acetate/heptane) and crystallization from dichloromethane/hexane

출처 및 근거

ORD 기록
ord-db581be9e9a645418ab15af626b7f361
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07238808B2

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