tert-Butanol → HCID 57564136, compound

HRID 501256Notes

Reaction equation

HRID 501256 reaction equation
[CH3:1][C:2]([OH:5])([CH3:4])[CH3:3].Cl[S:7]([N:10]=[C:11]=[O:12])(=[O:9])=[O:8].[CH:13]1([NH2:16])[CH2:15][CH2:14]1>C(Cl)Cl>[CH:13]1([NH:16][S:7]([NH:10][C:11](=[O:12])[O:5][C:2]([CH3:4])([CH3:3])[CH3:1])(=[O:9])=[O:8])[CH2:15][CH2:14]1

Participants

5

Reactant 3

HCID 6386tert-ButanolHCID 69828CyclopropylamineHCID 70918Chlorosulfonyl isocyanate

Product 1

HCID 57564136HCID 57564136, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.33 ml of t-BuOH were dissolved in 50 ml of anhydrous CH2Cl2 and, at RT, 2.00 g of chlorosulfonyl isocyanate were added dropwise. During this, the internal temperature rose to 30° C. Stirring at RT for 1 hour was followed by dropwise addition of 1.96 ml of cyclopropylamine and leaving the reaction mixture to stand at RT for 16 hours. It was then washed 3 times with 15 ml of water each time. After drying over Na2SO4, the solvent was removed in vacuo. 1.3 g of an amorphous solid were obtained.

Workup

  1. customrose to 30° C
  2. customleaving the reaction mixture
  3. waitto stand at RT for 16 hours
  4. washIt was then washed 3 times with 15 ml of water each time
  5. dry with materialAfter drying over Na2SO4
  6. customthe solvent was removed in vacuo

Sources & evidence

ORD record
ord-bb995ea2f7de4392a54bd0274586618b
Source dataset
uspto-grants-2010_08
Patent number
US07772262B2

Reaction notes

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