Succinic Acid → HCID 178457292, compound

HRID 2406154Notes

Reaction equation

[CH2:1]([N:4]([CH2:47][CH2:48][CH3:49])[C:5]([CH2:7][O:8][C:9](=[O:46])[CH2:10][CH2:11][NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([N:24]2[CH2:45][CH2:44][C:27]3([NH:31]/[C:30](=[N:32]/[C:33]([C:35]4[C:40]([NH2:41])=[N:39][C:38]([NH2:42])=[C:37]([Cl:43])[N:36]=4)=[O:34])/[NH:29][CH2:28]3)[CH2:26][CH2:25]2)=[O:23])[CH:17]=1)(=[O:15])=[O:14])=[O:6])[CH2:2][CH3:3].[C:50]([OH:57])(=[O:56])[CH2:51][CH2:52][C:53]([OH:55])=[O:54]>CO>[C:50]([OH:57])(=[O:56])[CH2:51][CH2:52][C:53]([OH:55])=[O:54].[CH2:47]([N:4]([CH2:1][CH2:2][CH3:3])[C:5]([CH2:7][O:8][C:9](=[O:46])[CH2:10][CH2:11][NH:12][S:13]([C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([C:22]([N:24]2[CH2:45][CH2:44][C:27]3([NH:31]/[C:30](=[N:32]/[C:33]([C:35]4[C:40]([NH2:41])=[N:39][C:38]([NH2:42])=[C:37]([Cl:43])[N:36]=4)=[O:34])/[NH:29][CH2:28]3)[CH2:26][CH2:25]2)=[O:23])[CH:17]=1)(=[O:15])=[O:14])=[O:6])[CH2:48][CH3:49]

Participants

Conditions

Temperature: 0 °C

Procedure

1 g of 3-(3-{2-[(E)-3,5-Diamino-6-chloro-pyrazine-2-carbonylimino]-1,3,8-triaza-spiro[4.5]decane-8-carbonyl}-benzenesulfonylamino)-propionic acid dipropylcarbamoylmethyl ester (may be prepared as in Preparation 1) and 0.18 g succinic acid were dissolved in 7.97 g methanol in a glass vial at 50° C. The solution was cooled to 0° C. and then stirred at that temperature for 24 hours. Afterwards, crystals were collected by filtration and dried at 60° C. and 1 mbar for 3 hours. Off-white to yellowish crystals of form C were obtained.

Workup

filtrationAfterwards, crystals were collected by filtration
customdried at 60° C.
wait1 mbar for 3 hours
customwere obtained

Sources & evidence

ORD record: ord-431737c4db604c6aba6d5d8d13667249
Source dataset: uspto-grants-2014_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08809340B2

Reaction notes

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