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Ammonium Chloride → tert-Butyl (4-{(1S,2R)-1-[(4-chlorophenyl)amino]-2-({[2-(4-chlorophenyl)-5,5-dimethyl 1,3-dioxan-2-yl]methyl}thio)-3-oxo-3-[(4S)-2-oxo-4-phenyl-1,3-oxazolidin-3-yl]propyl}phenoxy)acetate

HRID 254101
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HRID 254101 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH2:16][S:17][CH2:18][C:19]([N:21]3[C@@H:25]([C:26]4[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=4)[CH2:24][O:23][C:22]3=[O:32])=[O:20])[O:13][CH2:12][C:11]([CH3:15])([CH3:14])[CH2:10][O:9]2)=[CH:4][CH:3]=1.[Cl:33][C:34]1[CH:39]=[CH:38][C:37](/[N:40]=[CH:41]/[C:42]2[CH:56]=[CH:55][C:45]([O:46][CH2:47][C:48]([O:50][C:51]([CH3:54])([CH3:53])[CH3:52])=[O:49])=[CH:44][CH:43]=2)=[CH:36][CH:35]=1.C(N(C(C)C)C(C)C)C.[NH4+].[Cl-]>C(Cl)Cl.[Cl-].[Na+].O.CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].Cl[Ti](Cl)(Cl)Cl.C(O)(C)C>[Cl:33][C:34]1[CH:35]=[CH:36][C:37]([NH:40][C@@H:41]([C:42]2[CH:43]=[CH:44][C:45]([O:46][CH2:47][C:48]([O:50][C:51]([CH3:52])([CH3:53])[CH3:54])=[O:49])=[CH:55][CH:56]=2)[C@@H:18]([S:17][CH2:16][C:8]2([C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=3)[O:9][CH2:10][C:11]([CH3:14])([CH3:15])[CH2:12][O:13]2)[C:19](=[O:20])[N:21]2[C@@H:25]([C:26]3[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=3)[CH2:24][O:23][C:22]2=[O:32])=[CH:38][CH:39]=1
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참가 물질

10

반응물 4

HCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 66843329(4S)-3-[({[2-(4-Chlorophenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetyl]-4-phenyl-1,3-oxazolidin-2-oneHCID 178451334HCID 178451334, 화합물

생성물 1

HCID 86619096
tert-Butyl (4-{(1S,2R)-1-[(4-chlorophenyl)amino]-2-({[2-(4-chlorophenyl)-5,5-dimethyl 1,3-dioxan-2-yl]methyl}thio)-3-oxo-3-[(4S)-2-oxo-4-phenyl-1,3-oxazolidin-3-yl]propyl}phenoxy)acetate
수율 67.9%

시약·촉매·용매 5

HCID 11026Titanium isopropoxide촉매HCID 24193Titanium Tetrachloride촉매HCID 3776Isopropanol용매HCID 6344Dichloromethane용매3회HCID 57417360Sodium chloride; water용매

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온도
-40 °C

실험 절차

Tetraisopropyl orthotitanate (0.23 ml, 0.77 mmol) was added to a solution of TiCl4 (1M in CH2Cl2, 2.25 ml, 2.25 mmol) in CH2Cl2 (22 ml) at 0° C. under inert atmosphere. The mixture was stirred for ten minutes. (4S)-3-[({[2-(4-Chlorophenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetyl]-4-phenyl-1,3-oxazolidin-2-one (1.44 g, 3.03 mmol) in dry CH2Cl2 (25 ml) was added dropwise over 45 minutes and the mixture was stirred for ten minutes. tert-Butyl (4-{(E)-[(4-chlorophenyl)imino]methyl}phenoxy)acetate (2.09 g, 6.04 mmol) in dry CH2Cl2 (25 ml) was added dropwise over 80 minutes. The mixture was cooled to −40° C. and stirred for 20 minutes. Ethyl diisopropyl amine (1.03 ml, 6.02 mmol) was added dropwise over 40 minutes and the mixture was stirred at −40° C. for ten minutes. The mixture was cooled to −78° C. and isopropanol (80 ml) was added. The temperature was allowed to reach room temperature over three hours. NH4Cl (10%, 80 ml) was added and the mixture was stirred for 35 minutes. Brine (200 ml) was added and the mixture was extracted twice with 400 ml diethyl ether. The combined organic layers were dried (MgSO4) and concentrated under reduced pressure. Purification by flash-chromatography (10%-20% EtOAc in hexane) afforded 1.69 g (65%) of the title compound as a white solid. 1H-NMR (CDCl3, 200 MHz): δ 0.65 (s, 3H), 1.3 (s, 3H), 1.5 (s, 9H), 2.6-2.9 (m, 2H), 3.4 (m, 4H), 4.2 (m, 1H), 4.5 (s, 2H), 4.64-8 (m, 2H), 5.3 (m, 1H), 5.7 (d, 1H), 6.4 (m, 2H), 6.7-7.4 (m, 15H).

후처리

  1. stirringthe mixture was stirred for ten minutes
  2. stirringstirred for 20 minutes
  3. stirringthe mixture was stirred at −40° C. for ten minutes
  4. temperatureThe mixture was cooled to −78° C.
  5. stirringthe mixture was stirred for 35 minutes
  6. extractionthe mixture was extracted twice with 400 ml diethyl ether
  7. dry with materialThe combined organic layers were dried (MgSO4)
  8. concentrationconcentrated under reduced pressure
  9. customPurification by flash-chromatography (10%-20% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-bb6a0f2644be4caebc5eafb815c1a3f9
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07871998B2

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