Ammonium formate → HCID 19438536, compound

HRID 37059Notes

Reaction equation

HRID 37059 reaction equation
C([O:8][CH2:9][CH:10]1[CH2:21][NH:20][CH2:19][CH:18]([CH2:22][O:23]CC2C=CC=CC=2)[NH:17][CH2:16][CH2:15][S:14][CH2:13][CH2:12][NH:11]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.[Pd]>[OH:23][CH2:22][CH:18]1[CH2:19][NH:20][CH2:21][CH:10]([CH2:9][OH:8])[NH:11][CH2:12][CH2:13][S:14][CH2:15][CH2:16][NH:17]1

Participants

5

Reactant 2

HCID 2723923Ammonium formateHCID 194385495,9-Bis(benzyloxymethyl)-1-thia-4,7,10-triazacyclododecane

Product 1

HCID 19438536HCID 19438536, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Conditions

Temperature
50 °C

Procedure

5,9-Bis (benzyloxymethyl) -1-thia-4,7,10-triazacyclododecane (0.28 g, 0.65 mmol) was dissolved in methanol (10 ml). Ammonium formate (0.39 g) and 10% Palladium on carbon (1.3 g) were added under nitrogen and the mixture was stirred at 50° C. for 16 hours. The catalyst was filtered off and washed with methanol (5 ml). The filtrate was evaporated and 5,9-bis(hydroxymethyl)-1-thia-4,7,10-triazacyclododecane was isolated as a white solid. Mp. 210°-220° C. (subl.). Yield: 0.099 g (61%).

Workup

  1. filtrationThe catalyst was filtered off
  2. washwashed with methanol (5 ml)
  3. customThe filtrate was evaporated

Sources & evidence

ORD record
ord-04de0d936f4841db822f59d428b0c1b7
Source dataset
uspto-grants-1995_05
Patent number
US05419893

Reaction notes

Loading…