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Hydrochloric Acid → Agn-194310

HRID 2420656
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HRID 2420656 반응식
[OH-].[Na+].[CH2:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([C:21]#[C:22][C:23]4[CH:33]=[CH:32][C:26]([C:27]([O:29]CC)=[O:28])=[CH:25][CH:24]=4)[CH:19]=3)[S:14][C:13]([CH3:35])([CH3:34])[CH:12]=2)=[CH:7][CH:6]=1)[CH3:4].Cl>C1COCC1.C(O)C>[CH3:4][CH2:3][C:5]1[CH:6]=[CH:7][C:8]([C:11]2[C:20]3[CH:19]=[C:18]([C:21]#[C:22][C:23]4[CH:24]=[CH:25][C:26]([C:27]([OH:29])=[O:28])=[CH:32][CH:33]=4)[CH:17]=[CH:16][C:15]=3[S:14][C:13]([CH3:34])([CH3:35])[CH:12]=2)=[CH:9][CH:10]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21957874Ethyl 4-[[4-(4-ethylphenyl)-2,2-dimethyl-(2h)-thiochromen-6-yl]ethynyl]-benzoate

생성물 1

HCID 9867046Agn-194310

시약·촉매·용매 2

HCID 702Ethanol용매HCID 8028Tetrahydrofuran용매

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온도
40 °C

실험 절차

Two ml of a 2 M solution of NaOH were added to a solution of ethyl 4[[4-(4-ethylphenyl)-2,2-dimethyl-[2H]-thiochromen-6-yl]-ethynyl]benzoate in THF and ethanol. The solution was heated to 40° C., stirred overnight, then cooled to room temperature. The reaction mixture was acidified with 1 N HCl (4 ml). At the beginning of the process, the reaction mixture formed a heterogeneous system. The mixture was extracted with ethyl acetate (25 ml×2). The combined organic layers were washed with 10 ml water, saturated aqueous NaCl, and dried with NaSO4, and the solvent was removed under reduced pressure. The residual solid (0.31 gram) was recrystallized from acetonitrile (25 ml) to yield 4-[[4-(4-ethylphenyl)-2,2-dimethyl-(2H)-thiochroman-6-yl]-ethynyl]benzoic acid, (AGN194310) (0.236 gram, 70%) as a colorless solid (m.p. 210-212° C.) [1H-NMR (DMSO-d6): d8.2 (s, 2H), d7.8 (s, 2H), d7.6 (s, 2H), d7.4 (s, 2H), d7.2 (s, 2H), d7.0 (s, 1H), d6.0 (s, 1H), d2.6 (t, 2H, J=35 Hz), d1.6 (s, 6H), d1.4 (t, 3H, J=46 Hz)].

후처리

  1. temperaturecooled to room temperature
  2. customAt the beginning of the process, the reaction mixture formed a heterogeneous system
  3. extractionThe mixture was extracted with ethyl acetate (25 ml×2)
  4. washThe combined organic layers were washed with 10 ml water, saturated aqueous NaCl
  5. dry with materialdried with NaSO4
  6. customthe solvent was removed under reduced pressure
  7. customThe residual solid (0.31 gram) was recrystallized from acetonitrile (25 ml)

출처 및 근거

ORD 기록
ord-b4d679c73b1d46e59035db9db3ae5583
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07955852B2

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