Carbon Dioxide → Solvent Red 49

HRID 2295700

반응식

HRID 2295700 반응식
[CH3:1][CH2:2][N:3]([C:6]1[CH:7]=[CH:8][C:9]2[C:24]([C:25]3[CH:26]=[CH:27][CH:28]=[CH:29][C:30]=3[C:31](C)=[O:32])=[C:23]3[C:13](=[CH:14][C:15]([CH:21]=[CH:22]3)=[N+:16]([CH2:19][CH3:20])[CH2:17][CH3:18])[O:12][C:10]=2[CH:11]=1)[CH2:4][CH3:5].C(N(CC)C1C=C([OH:43])C=CC=1)C.C1(=O)OC(=O)C2=CC=CC=C12.C(=O)=O.[OH-].[Na+]>O>[CH3:5][CH2:4][N:3]([C:6]1[CH:7]=[CH:8][C:9]2[C:24]3([O:32][C:31](=[O:43])[C:30]4[C:25]3=[CH:26][CH:27]=[CH:28][CH:29]=4)[C:23]3[CH:22]=[CH:21][C:15]([N:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][C:13]=3[O:12][C:10]=2[CH:11]=1)[CH2:2][CH3:1]

참가 물질

7

반응물 5

HCID 280Carbon DioxideHCID 6811Phthalic AnhydrideHCID 70623-(Diethylamino)phenolHCID 14798Sodium HydroxideHCID 45271881[9-(2-Acetylphenyl)-6-(diethylamino)xanthen-3-ylidene]-diethylazanium

생성물 1

HCID 62357Solvent Red 49수율 90%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

The Rhodamine dye of formula (II), Rhodamine B free base (Colour Index 45170:1), a well-known pigment, can be prepared by heating a stirred mixture of 10 parts by weight of m-diethylaminophenol and 12 parts by weight of phthalic anhydride to 175° C. under a blanket of carbon dioxide. The reaction mixture is stirred at 170°-175° C. for a period of 6-7 hours, then cooled to 40° C. and discharged into water. The pH of the resulting slurry is adjusted to 12 by adding caustic soda, and the insoluble material is recovered by filtration. The filter cake is then rinsed with water and dried to obtain Rhodamine B Base in a yield about 90% of theoretical.

후처리

  1. temperatureby heating
  2. filtrationthe insoluble material is recovered by filtration
  3. washThe filter cake is then rinsed with water
  4. customdried

출처 및 근거

ORD 기록
ord-ed8de1c0e85242978067f03c34f2e41e
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04426205

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