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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
Notes
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Reaction equation

HRID 254101 reaction equation
[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
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

10

Reactant 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, compound

Product 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
Yield 67.9%

Reagents, catalysts & solvents 5

HCID 11026Titanium isopropoxideCatalystHCID 24193Titanium TetrachlorideCatalystHCID 3776IsopropanolSolventHCID 6344DichloromethaneSolvent3×HCID 57417360Sodium chloride; waterSolvent

Conditions

Temperature
-40 °C

Procedure

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).

Workup

  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)

Sources & evidence

ORD record
ord-bb6a0f2644be4caebc5eafb815c1a3f9
Source dataset
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07871998B2

Reaction notes

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