Sulfamide → HCID 86657941, compound

HRID 1186446Notes

Reaction equation

HRID 1186446 reaction equation
[C:1]([NH:8][CH2:9][CH2:10][NH2:11])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[S:12](N)([NH2:15])(=[O:14])=[O:13]>O1CCCC1>[C:4]([O:3][C:1]([NH:8][CH2:9][CH2:10][NH:11][S:12](=[O:14])(=[O:13])[NH2:15])=[O:2])([CH3:5])([CH3:6])[CH3:7]

Participants

4

Reactant 2

HCID 82267SulfamideHCID 187201N-BOC-ethylenediamine

Product 1

HCID 86657941HCID 86657941, compoundYield 50%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Conditions

Temperature
100 °C

Procedure

According to Reference Example 9-26, tetrahydrofuran (3 mL) and N—BOC-ethylenediamine (0.66 mL, 4.2 mmol) were added to sulfamide (400 mg, 4.2 mmol) and the mixture was stirred by use of a microwave chemical reactor at 300 W at 100° C. for 10 minutes. The solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=1/0 to 9/1) was performed to give N-[2-(tert-butoxycarbonylamino)ethyl]-sulfuric diamide (Compound GJ) (500 mg, yield: 50%).

Workup

  1. customThe solvent was evaporated off under reduced pressure, and purification by silica gel column chromatography (chloroform/methanol=1/0 to 9/1)

Sources & evidence

ORD record
ord-7a0bbc2c39204f6b9ae56ded58f424ac
Source dataset
uspto-grants-2014_03
Patent number
US08673908B2

Reaction notes

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