Sodium Sulfate → HCID 67072554, compound

HRID 1948164Notes

Reaction equation

[CH2:1]([Mg]Cl)[CH3:2].[C:5]([Si:9]([CH3:30])([CH3:29])[O:10][CH:11]1[CH2:16][CH2:15][C:14]([CH:21]=[N:22][S:23]([C:25]([CH3:28])([CH3:27])[CH3:26])=[O:24])([C:17]([F:20])([F:19])[F:18])[CH2:13][CH2:12]1)([CH3:8])([CH3:7])[CH3:6].[O-]S([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[C:5]([Si:9]([CH3:30])([CH3:29])[O:10][CH:11]1[CH2:12][CH2:13][C:14]([CH:21]([NH:22][S:23]([C:25]([CH3:28])([CH3:27])[CH3:26])=[O:24])[CH2:1][CH3:2])([C:17]([F:19])([F:20])[F:18])[CH2:15][CH2:16]1)([CH3:8])([CH3:7])[CH3:6]

Participants

Conditions

Temperature: -78 °C

Procedure

13.4 ml (26.8 mmol) of a 2M solution of ethylmagnesium chloride in diethyl ether were diluted using 8 ml of anhydrous diethyl ether and cooled to −78° C. At that temperature, a solution of 3.7 g (8.95 mmol) of 2-methyl-propane-2-sulfinic acid 1-[4-(tert-butyl-dimethyl-silanyloxy)-1-trifluoromethyl-cyclohexyl]methylideneamide (72) in anhydrous diethyl ether was added dropwise. Afterwards, the mixture was allowed to warm to ambient temperature and was stirred for 2 h at ambient temperature. 100 ml of a saturated aqueous Na2SO4-solution was added, the organic layer separated, dried using MgSO4 and evaporated to give 3.22 g of 73 as an oil, used without further purification. Rt=1.09 min (Method Q).

Workup

temperatureto warm to ambient temperature
customthe organic layer separated
customdried
customevaporated

Sources & evidence

ORD record: ord-7b62317794e040aba0dd881ab6efabcb
Source dataset: uspto-grants-2013_03
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08399482B2

Reaction notes

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