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Triethylamine → HCID 178456931, 화합물

HRID 1620613
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HRID 1620613 반응식
C(N(CC)CC)C.[CH:8]([C:10]1[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([C:18]([F:21])([F:20])[F:19])[CH:11]=1)=O.Cl.Cl.[NH:24]1[CH2:29][CH2:28][CH:27](/[CH:30]=[C:31]2/[C:32]([NH:37][CH2:38][C:39]#[CH:40])=[N:33][C:34](=[O:36])[S:35]/2)[CH2:26][CH2:25]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CN(C=O)C.O>[O:36]=[C:34]1[N:33]=[C:32]([NH:37][CH2:38][C:39]#[CH:40])/[C:31](=[CH:30]/[CH:27]2[CH2:26][CH2:25][N:24]([CH2:8][C:10]3[CH:17]=[CH:16][C:13]([C:14]#[N:15])=[C:12]([C:18]([F:21])([F:20])[F:19])[CH:11]=3)[CH2:29][CH2:28]2)/[S:35]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 199588974-Formyl-2-(trifluoromethyl)benzonitrileHCID 178456897HCID 178456897, 화합물

생성물 1

HCID 178456931HCID 178456931, 화합물수율 23.3%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of triethylamine (1.38 mL) and 4-formyl-2-(trifluoromethyl)benzonitrile (593 mg) in DMF (10 mL) was added (5Z)-5-(piperidin-4-ylmethylidene)-4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one dihydrochloride (800 mg). The reaction mixture was stirred at room temperature for 1 hr, and sodium triacetoxyborohydride (2.1 g) was added. The reaction mixture was stirred at room temperature for 3 hr, water was added, and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) and recrystallized from ethyl acetate/heptane to give the title compound (250 mg).

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 3 hr
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)
  7. customrecrystallized from ethyl acetate/heptane

출처 및 근거

ORD 기록
ord-5126a03b89e9476c9ce6edc69033e881
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772277B2

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