Water → HCID 178421808、化合物

HRID 728352

反応式

HRID 728352 の反応式
[C:1]1([C:3](=[CH:5][C:6](=[CH:8][CH:9]=1)[CH3:7])[CH3:4])C.[F:10][C:11]([F:24])([F:23])[CH2:12][CH2:13][NH:14][C:15]1[CH:16]=[C:17]([OH:22])[CH:18]=[CH:19][C:20]=1[CH3:21].[OH-:25].[Na+].[OH2:27]>>[OH-:22].[C:21]([C:20]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[C:7]1[C:18]2[C:17]([O+:22]=[C:8]3[C:6]=1[CH:5]=[C:3]([CH3:4])[C:1]([NH:14][CH2:13][CH2:12][C:11]([F:10])([F:24])[F:23])=[CH:9]3)=[CH:16][C:15]([NH:14][CH2:13][CH2:12][C:11]([F:23])([F:24])[F:10])=[C:20]([CH3:21])[CH:19]=2)([OH:27])=[O:25]

参加物

5

反応物 4

HCID 962WaterHCID 72471,2,4-TrimethylbenzeneHCID 14798Sodium HydroxideHCID 543497383-Trifluoropropylamino-4-methylphenol

生成物 1

HCID 178421808HCID 178421808、化合物

反応条件

温度
100 °C

実験手順

The pseudocumene layer from alkylation, containing 0.35-0.38 mole of 3-trifluoropropylamino-4-methylphenol was refluxed in a 1 L 3-necked flask fitted with thermometer, stirrer and Dean-Stark trap in order to remove water as the azeotrope. To the dry solution was added 30 g of phthalic anhydride. Condensation was effected by heating at reflux for 20 hours while removing water generated by reaction as the pseudocumene-water azeotrope. The solution turned red. When condensation was complete the solution was cooled to 100° C., 300 ml water and 25 g 50% sodium hydroxide added, and the pseudocumene removed by azeotropic distillation. The red dye which had crystallized out was separated by filtration and washed with 400 ml water (142 g wet paste). This filtercake was reslurried in 400 ml water and 10 g 50% sodium hydroxide, heated 30 minutes at 100° C., filtered again and washed with 400 ml water. Upon drying at 100° C., 40 g of dye zwitterion was obtained which melted at 258°-260° C.

後処理

  1. temperaturewas refluxed in a 1 L 3-necked flask
  2. customfitted with thermometer, stirrer and Dean-Stark trap in order
  3. customto remove water as the azeotrope
  4. additionTo the dry solution was added 30 g of phthalic anhydride
  5. customCondensation
  6. temperatureby heating
  7. temperatureat reflux for 20 hours
  8. customwhile removing water
  9. customgenerated by reaction as the pseudocumene-water azeotrope
  10. customWhen condensation
  11. customthe pseudocumene removed by azeotropic distillation
  12. customThe red dye which had crystallized out
  13. customwas separated by filtration
  14. washwashed with 400 ml water (142 g wet paste)
  15. temperature10 g 50% sodium hydroxide, heated 30 minutes at 100° C.
  16. filtrationfiltered again
  17. washwashed with 400 ml water
  18. customUpon drying at 100° C.
  19. custom40 g of dye zwitterion was obtained which melted at 258°-260° C.

出典と根拠

ORDレコード
ord-7f31f22035324278a49305eb62f7d50f
出典データセット
uspto-grants-1991_09
特許番号
US05047559

関連ノート

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