Methane → 2,2',2''-(10-(1,3,4-Trihydroxybutan-2-yl)-1,4,7,10-tetraazacyclododecane-1,4,7-triyl)triacetic acid

HRID 63024Notes

Reaction equation

C(=O)([O-])[O-].[Ca+2].[CH2:6]1[N:17]([CH2:18][C:19]([OH:21])=[O:20])[CH2:16][CH2:15][N:14]([CH2:22][C:23]([OH:25])=[O:24])[CH2:13][CH2:12][N:11]([C@@H:26]([C@H:29]([OH:32])[CH2:30][OH:31])[CH2:27][OH:28])[CH2:10][CH2:9][N:8]([CH2:33][C:34]([OH:36])=[O:35])[CH2:7]1.C>O>[CH2:6]1[N:17]([CH2:18][C:19]([OH:21])=[O:20])[CH2:16][CH2:15][N:14]([CH2:22][C:23]([OH:25])=[O:24])[CH2:13][CH2:12][N:11]([CH:26]([CH:29]([OH:32])[CH2:30][OH:31])[CH2:27][OH:28])[CH2:10][CH2:9][N:8]([CH2:33][C:34]([OH:36])=[O:35])[CH2:7]1

Participants

Conditions

Temperature: 90 °C

Procedure

A total of 3.356 kg calcium carbonate (99.3%) is added in portions to 15.39 kg butrol (water contents: 2.6%) dissolved in 120 l demineralised water and it is stirred for one hour at 90° C. inner temperature. It is subsequently cooled to 20° C. and 1.5 kg active carbon (Norit SX PLUS; the carbon is first washed thoroughly with water) is added. It is stirred for one hour at 20° C. and the carbon is subsequently filtered off. The carbon is washed three times with 15 l of water each time.

Workup

dissolutiondissolved in 120 l
temperatureIt is subsequently cooled to 20° C.
washthe carbon is first washed thoroughly with water)
additionis added
stirringIt is stirred for one hour at 20° C.
filtrationthe carbon is subsequently filtered off
washThe carbon is washed three times with 15 l of water each time

Sources & evidence

ORD record: ord-ccde40df819d4a679b4244e8c2673f05
Source dataset: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09447053B2

Reaction notes

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