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Toluene → (R)-4-chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine-5-oxide

HRID 243639
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HRID 243639 반응식
C1([C@@H](C(C2C=CC=CC=2)O)[OH:8])C=CC=CC=1.C1(C)C=CC=CC=1.[Cl:24][C:25]1[C:26]2[S:46][CH2:45][CH2:44][C:27]=2[N:28]=[C:29]([N:31]2[CH2:36][CH2:35][N:34]([C:37]3[CH:42]=[CH:41][C:40]([Cl:43])=[CH:39][CH:38]=3)[CH2:33][CH2:32]2)[N:30]=1.CC(OO)(C)C>O>[Cl:24][C:25]1[C:26]2[S@:46](=[O:8])[CH2:45][CH2:44][C:27]=2[N:28]=[C:29]([N:31]2[CH2:32][CH2:33][N:34]([C:37]3[CH:38]=[CH:39][C:40]([Cl:43])=[CH:41][CH:42]=3)[CH2:35][CH2:36]2)[N:30]=1
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6

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HCID 1140TolueneHCID 6410tert-Butyl hydroperoxideHCID 594759174-Chloro-2-[4-(4-chlorophenyl)piperazin-1-yl]-6,7-dihydrothieno[3,2-d]pyrimidineHCID 68495654(s)-Hydrobenzoin

생성물 1

HCID 86645100(R)-4-chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine-5-oxide수율 88%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

Using a jacketed reactor with mechanical stirring at 400 rpm, charge (S)-Hydrobenzoin (292 mg) and toluene (50 mL), followed by Ti(i-PrO)4 (0.20 mL) and water (0.25 mL). Stir the mixture at 20° C. for 30 min. then charge 4-Chloro-2-[4-(4-chloro-phenyl)-piperazin-1-yl]-6,7-dihydro-thieno[3,2-d]pyrimidine (3a, 5.00 g) and stir the mixture for 15 min at 20° C. before being cooling to 0° C. (it took 20 min). Charge TBHP (70% aqueous) (0.75 mL) to the reaction mixture and stir for 23 h at 0° C. Reaction reached 96% conversion and 89% ee. Quench with 5% Na2SO3 (20 mL). Separate the layers and extract the aqueous layer with dichloromethane (50 mL). Combine organic layers and wash with water (20 mL), dry (MgSO4), filter, and concentrate affording the desired sulfoxide in (4.6 g, 88% yield, 89% ee). The product may be recrystallized from THF/water (5:1) with good recovery to yield material >96% ee. NMR (400 MHz, CDCl3) δ 7.16-7.26 (m, 2H), 6.80-6.90 (m, 2H), 3.90-4.20 (m, 4H), 3.75-3.90 (m, 1H), 3.00-3.30 (m, 7H); 13C NMR (400 MHz, CDCl3) δ 177.5, 162.5, 160.7, 149.8, 129.4, 125.7, 123.9, 118.2, 49.6, 46.5, 44.7, 44.4, 33.7 (3 signals missing due to overlap); LCMS (ESI) for C16H17Cl2N4OS (M+H)+: calcd. 383.1, obsvd. 383.0.

후처리

  1. stirringStir the mixture at 20° C. for 30 min.
  2. customReaction
  3. customQuench with 5% Na2SO3 (20 mL)
  4. customSeparate the layers
  5. extractionextract the aqueous layer with dichloromethane (50 mL)
  6. washCombine organic layers and wash with water (20 mL)
  7. dry with materialdry (MgSO4)
  8. filtrationfilter
  9. concentrationconcentrate

출처 및 근거

ORD 기록
ord-3402bee756b44a5ba841e39881356923
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653282B2

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