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Hexachloroethane → Diethyl-carbamic acid 1-(tert-butyl-dimethyl-silanyl)-4-chloro-1H-indol-5-yl ester

HRID 45143
Notes
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Reaction equation

HRID 45143 reaction equation
[C:1]([Si:5]([CH3:24])([CH3:23])[N:6]1[C:14]2[C:9](=[CH:10][C:11]([O:15][C:16](=[O:22])[N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])=[CH:12][CH:13]=2)[CH:8]=[CH:7]1)([CH3:4])([CH3:3])[CH3:2].CN(CCN(C)C)C.C([Li])(CC)C.[Cl:38]C(Cl)(Cl)C(Cl)(Cl)Cl.[Cl-].[NH4+]>C1COCC1>[C:1]([Si:5]([CH3:24])([CH3:23])[N:6]1[C:14]2[C:9](=[C:10]([Cl:38])[C:11]([O:15][C:16](=[O:22])[N:17]([CH2:20][CH3:21])[CH2:18][CH3:19])=[CH:12][CH:13]=2)[CH:8]=[CH:7]1)([CH3:2])([CH3:3])[CH3:4]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

HCID 6214HexachloroethaneHCID 8037N,N,N',N'-TetramethylethylenediamineHCID 25517Ammonium ChlorideHCID 9975323Diethyl-carbamic acid 1-(tert-butyl-dimethyl-silanyl)-1H-indol-5-yl esterHCID 178418400CID 53628100

Product 1

HCID 9977109
Diethyl-carbamic acid 1-(tert-butyl-dimethyl-silanyl)-4-chloro-1H-indol-5-yl ester

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent2×

Conditions

Temperature
-78 °C

Procedure

Diethyl-carbamic acid 1-(tert-butyl-dimethyl-silanyl)-1H-indol-5-yl ester (9.26 g, 26.7 mmol) is dissolved in THF (250 mL), flushed with nitrogen and cooled to −78° C. TMEDA (5 mL, 33.1 mmol) is then added followed by sec-butyllithium (24.8 mL, 34.7 mmol) and the reaction is stirred for 30 minutes. Hexachloroethane (12.73 g, 53.8 mmol) in 50 mL of THF is added over 10 minutes to the reaction. The reaction is allowed to warm to room temperature overnight (15 hours). The reaction is cooled using an ice bath and a saturated ammonium chloride (aq) solution is added (150 mL). The mixture is then extracted with ethyl acetate, dried (sodium sulfate) and concentrated to obtain the title compound as an oil that is used without further purification. MS (ESI) m/z 381.1 (M+1).

Workup

  1. customflushed with nitrogen
  2. temperatureto warm to room temperature overnight (15 hours)
  3. temperatureThe reaction is cooled
  4. extractionThe mixture is then extracted with ethyl acetate
  5. dry with materialdried (sodium sulfate)
  6. concentrationconcentrated

Sources & evidence

ORD record
ord-1f12c182fb30481e9d63de934582b7f4
Source dataset
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08541432B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes