Hydrochloric Acid → HCID 86664465, compound

HRID 445235Notes

Reaction equation

[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:41]=[CH:40][C:18]([CH2:19][N:20]2[C@H:24]([C:25]([O:27]CC)=[O:26])[CH2:23][C:22]3([CH2:34][CH2:33][N:32]([CH:35]([CH2:38][CH3:39])[CH2:36][CH3:37])[CH2:31][CH2:30]3)[CH2:21]2)=[CH:17][CH:16]=1)[CH2:8][C:9]1[NH:10][CH:11]=[CH:12][N:13]=1.[OH-].[Na+].Cl.[Cl-].[Ca+2:46].[Cl-]>C(O)C.O>[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:19][N:20]2[C@H:24]([C:25]([OH:27])=[O:26])[CH2:23][C:22]3([CH2:34][CH2:33][N:32]([CH:35]([CH2:36][CH3:37])[CH2:38][CH3:39])[CH2:31][CH2:30]3)[CH2:21]2)=[CH:40][CH:41]=1)[CH2:8][C:9]1[NH:13][CH:12]=[CH:11][N:10]=1.[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[CH2:6][N:7]([CH2:14][C:15]1[CH:16]=[CH:17][C:18]([CH2:19][N:20]2[C@H:24]([C:25]([OH:27])=[O:26])[CH2:23][C:22]3([CH2:34][CH2:33][N:32]([CH:35]([CH2:36][CH3:37])[CH2:38][CH3:39])[CH2:31][CH2:30]3)[CH2:21]2)=[CH:40][CH:41]=1)[CH2:8][C:9]1[NH:13][CH:12]=[CH:11][N:10]=1.[Ca:46]

Participants

Conditions

Temperature: 70 °C

Procedure

The compound (16.5 g) obtained in Example 31(1) was dissolved in 52 mL of ethanol and an aqueous 2N sodium hydroxide solution (10 mL) was added thereto, followed by stirring at 70° C. for 2 hours. After completion of the reaction, the reaction solution was neutralized by adding an aqueous 5N hydrochloric acid solution (5.2 mL). To a separately prepared water 130 mL solution of calcium chloride (1.45 g), the neutralized solution was slowly added at 0° C., and the precipitated solid was filtered and washed with ethanol and water to obtain the title compound (14.2 g) having the following physical properties.

Workup

customAfter completion of the reaction
filtrationthe precipitated solid was filtered
washwashed with ethanol and water

Sources & evidence

ORD record: ord-523d803be9904e8c8f342146dddfcb6d
Source dataset: uspto-grants-2013_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08476290B2

Reaction notes

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