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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
ノート
印刷プレビュー

反応式

HRID 243639 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3402bee756b44a5ba841e39881356923
出典データセット
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08653282B2

反応ノート

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