Ammonia → HCID 20233207、化合物

HRID 65545

反応式

HRID 65545 の反応式
C1(O)C=CC=CC=1.B(O)(O)O.[CH2:12]([NH:28][C:29]1[C:42]2[C:41](=[O:43])[C:40]3[C:35](=[C:36](O)[CH:37]=[CH:38][C:39]=3[NH2:44])[C:34](=[O:46])[C:33]=2[C:32]([OH:47])=[CH:31][CH:30]=1)[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].[NH2:48]C1C2C(=O)C3C(=C(O)C=CC=3[N+]([O-])=O)C(=O)C=2C(O)=CC=1.C(Cl)CCCCCCCCCCCCCCC.O.NN.N>[N+](C1C=CC=CC=1)([O-])=O.CO.O.C1(C)C=CC=CC=1>[NH2:44][C:39]1[C:40]2[C:41](=[O:43])[C:42]3[C:33](=[C:32]([OH:47])[CH:31]=[CH:30][C:29]=3[NH:28][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[C:34](=[O:46])[C:35]=2[C:36]([NH2:48])=[CH:37][CH:38]=1

参加物

12

反応物 7

HCID 222AmmoniaHCID 996PhenolHCID 7628Boric AcidHCID 209931-ChlorohexadecaneHCID 24654Hydrazine hydrate (1:1)HCID 54840799,10-Anthracenedione, 1-amino-4,5-dihydroxy-8-nitro-HCID 20233208HCID 20233208、化合物

生成物 1

HCID 20233207HCID 20233207、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 1140Toluene溶媒HCID 7416Nitrobenzene溶媒

反応条件

温度
110 °C

実験手順

120 parts of phenol, 6.1 parts (0.1 mole) of boric acid and 70 parts of toluene are refluxed, while stirring, the water of reaction formed thereby being removed from the system. The toluene is then distilled off, the mixture is cooled to 110° C. and 25.4 parts (0.05 mole) of 1-palmitylamino-8-amino-4,5-dihydroxyanthraquinone (prepared by reacting 1-amino-8-nitro-4,5-dihydroxyanthraquinone with palmityl chloride in nitrobenzene and then reducing the product with hydrazine hydrate) are added. Ammonia is then passed in at this temperature until no further starting material can be detected in the thin-layer chromatogram (duration: 3 hours). The reaction mixture is cooled to 90° C. and 240 parts of methanol are added. After cooling to room temperature, the dye precipitated is filtered off with suction and the material on the filter is washed with methanol and water and dried. 20 parts of 1,4-diamino-5-hydroxy-8-palmitylaminoanthraquinone of melting point 174° C. are obtained.

後処理

  1. customformed
  2. customthereby being removed from the system
  3. distillationThe toluene is then distilled off
  4. additionare added
  5. temperatureThe reaction mixture is cooled to 90° C.
  6. temperatureAfter cooling to room temperature
  7. customthe dye precipitated
  8. filtrationis filtered off with suction
  9. washthe material on the filter is washed with methanol and water
  10. customdried

出典と根拠

ORDレコード
ord-e81c7b4ace6c436c8bde44d85e7a56a3
出典データセット
uspto-grants-1986_09
特許番号
US04614804

関連ノート

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