Hydrochloric Acid → Glycoluril

HRID 461758

反応式

HRID 461758 の反応式
CO.Cl.C(O)[N:5]1[C:9](=[O:10])[N:8](CO)[CH:7]2[N:13](CO)[C:14]([N:16](CO)[CH:6]12)=[O:15].C(=O)(O)[O-].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>>[CH:7]12[NH:13][C:14](=[O:15])[NH:16][CH:6]1[NH:5][C:9]([NH:8]2)=[O:10]

参加物

6

反応物 5

HCID 313Hydrochloric AcidHCID 887MethanolHCID 10340Sodium CarbonateHCID 79372Tetramethylolglycoluril2 回HCID 516892Sodium Bicarbonate

生成物 1

HCID 62347Glycoluril

実験手順

Into a suitable reaction vessel equipped with a stirrer, thermometer, and reflux condenser there was introduced 950 parts (30 moles) of methanol and 40 parts of concentrated hydrochloric acid. To this mixture, 262 parts (1 mole of tetramethylol glycoluril) were added and the reaction mixture was stirred at 25°-30° C. In about 15-20 minutes, all the tetramethylol glycoluril went into solution. After half an hour, the reaction mixture was neutralized with 140 parts of sodium bicarbonate and 20 parts of sodium carbonate at 22°-23° C. The pH after neutralization was about 8. The salt was filtered. The filtrate was concentrated at 60° C. under reduced pressure. The yield of the syrupy product after filtration of the salt was 290 parts, which was diluted to 90% solids with cellosolve. The product characteristics were as follows: Foil Solids: 91.4%; Pan Solids: 82.2%; and Gardner-Holdt Viscosity (25° C.): Z1. I.R. of the product indicated that the methylated product has a significant amount of unreacted methylol groups.

後処理

  1. customInto a suitable reaction vessel equipped with a stirrer
  2. temperaturethermometer, and reflux condenser
  3. waitAfter half an hour
  4. filtrationThe salt was filtered
  5. concentrationThe filtrate was concentrated at 60° C. under reduced pressure
  6. filtrationThe yield of the syrupy product after filtration of the salt
  7. additionwas diluted to 90% solids with cellosolve
  8. customGardner-Holdt Viscosity (25° C.)

出典と根拠

ORDレコード
ord-e605b185a2ee41e0909b660ab234a90d
出典データセット
uspto-grants-1977_12
特許番号
US04064191

関連ノート

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