Potassium hydroxy sulfite → HCID 71262248, compound

HRID 540257Notes

Reaction equation

HRID 540257 reaction equation
OO[S:3]([O-:5])=O.[K+].S1[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[CH2:11][N:10]([C:18]2[N:27]=[C:26]([NH:28][CH2:29][CH2:30][NH:31][C:32](=[O:38])[O:33][C:34]([CH3:37])([CH3:36])[CH3:35])[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([CH3:39])[CH:24]=3)[N:19]=2)[CH2:9][CH2:8]1>O.CO>[O:5]=[S:3]1[C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[CH2:11][N:10]([C:18]2[N:27]=[C:26]([NH:28][CH2:29][CH2:30][NH:31][C:32](=[O:38])[O:33][C:34]([CH3:36])([CH3:35])[CH3:37])[C:25]3[C:20](=[CH:21][CH:22]=[C:23]([CH3:39])[CH:24]=3)[N:19]=2)[CH2:9][CH2:8]1

Participants

5

Reactant 2

HCID 23707502Potassium hydroxy sulfiteHCID 86691424HCID 86691424, compound

Product 1

HCID 71262248HCID 71262248, compoundYield 128.7%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

To a solution of oxone (120 mg, 0.200 mmol) in water (0.7 mL) which was cooled below 0° C. in an ice bath, was added a solution of tert-butyl {2-[2-(2,3-dihydro-1,4-benzothiazepin-4(5H)-yl)-6-methylquinazolin-4-yl]aminoethyl}carbamate (155 mg, 0.333 mmol) in methanol (3 mL) dropwise. The mixture was stirred below 0° C. about 20 minutes. The formed precipitate was collected by filtration, washed with water and purified by flash column chromatography to afford 124 mg of the product as a white solid (yield was 77%).

Workup

  1. filtrationThe formed precipitate was collected by filtration
  2. washwashed with water
  3. custompurified by flash column chromatography

Sources & evidence

ORD record
ord-ce850226b11b4d7eaab5e6af7d6c90b6
Source dataset
uspto-grants-2014_10
Patent number
US08871756B2

Reaction notes

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