Hydrochloric Acid → HCID 178488026、化合物

HRID 593245

反応式

HRID 593245 の反応式
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[C:7]([NH2:12])[CH:6]=1.[C:13](O)(=[O:17])[C:14](O)=[O:15].Cl>>[CH3:3][O:4][C:5]1[CH:6]=[C:7]2[C:8](=[CH:9][CH:10]=1)[N:11]=[C:14]([OH:15])[C:13]([OH:17])=[N:12]2

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 971Oxalic AcidHCID 30851614-Methoxybenzene-1,2-diamine dihydrochloride2 回

生成物 1

HCID 178488026HCID 178488026、化合物

反応条件

温度
90 °C

実験手順

In a 50 L flask equipped with a mechanical stirrer, thermocouple and condenser was added 4-methoxy-1,2-phenylenediamine dihydrochloride salt (Compound 9) (2.65 kg @ 98 wt %, 12.30 mol), oxalic acid (1.582 kg @ 98 wt. %, 17.22 mol) and 3 N HCl(aq) (17.8 L) under nitrogen. The grey heterogeneous slurry was heated to 90° C. with steam for 7.25 hours. The reaction was monitored by HPLC. The resulting grey slurry was then cooled to an internal temperature of 20° C. overnight. The slurry was filtered, water (1.0-1.5 L/Kg) was used to help with the transfer. The light grey solids were washed with 2 cake volumes water (5.0-5.5 L/Kg). The solids were dried under vacuum/N2 sweep for 24 hours, at which time the solids were still very wet. The product was then slurry washed with methanol, and dried over 48 hours at 40-45° C. in a vacuum oven to give Compound 10 as an off-white product of 99.95% purity by HPLC assay. There was no methanol by NMR and the KF=0.05 wt. % water.

後処理

  1. customIn a 50 L flask equipped with a mechanical stirrer
  2. temperatureThe resulting grey slurry was then cooled to an internal temperature of 20° C. overnight
  3. filtrationThe slurry was filtered
  4. washThe light grey solids were washed with 2 cake volumes water (5.0-5.5 L/Kg)
  5. dry with materialThe solids were dried under vacuum/N2 sweep for 24 hours, at which time the solids
  6. washThe product was then slurry washed with methanol
  7. customdried over 48 hours at 40-45° C. in a vacuum oven

出典と根拠

ORDレコード
ord-2a10feb514cd4734a5bf598b0193ff36
出典データセット
uspto-grants-2016_01
特許番号
US09242917B2

関連ノート

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