Hydrochloric Acid → HCID 178507708, 화합물

HRID 1262494

반응식

HRID 1262494 반응식
ClCl.[CH:3]1[CH:8]=[C:7]2[C:9]([OH:20])=[C:10]3[C:15](=[C:16]([OH:17])[C:6]2=[CH:5][CH:4]=1)[C:14]([NH2:18])=[CH:13][CH:12]=[C:11]3[NH2:19].OS(O)(=O)=O.Cl.[NH2:27][C:28]1[C:41]2[C:40](=[O:42])[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:33](=[O:43])[C:32]=2[CH:31]=[CH:30][CH:29]=1.[K]>O>[CH:3]1[CH:8]=[C:7]2[C:9]([C:10]3[C:15]([C:16](=[O:17])[C:6]2=[CH:5][CH:4]=1)=[C:14]([NH:18][C:31]1[CH:30]=[CH:29][C:28]([NH2:27])=[C:41]2[C:40]([C:39]4[C:34]([C:33](=[O:43])[C:32]=12)=[CH:35][CH:36]=[CH:37][CH:38]=4)=[O:42])[CH:13]=[CH:12][C:11]=3[NH2:19])=[O:20]

참가 물질

8

반응물 6

HCID 313Hydrochloric AcidHCID 1118Sulfuric AcidHCID 67101-AminoanthraquinoneHCID 214029,10-Anthracenediol, 1,4-diamino-HCID 24526Chlorine2회HCID 5462222Potassium

생성물 1

HCID 178507708HCID 178507708, 화합물수율 103.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Chlorine is passed into a solution of 52.0 g of leuco-1,4-diaminoanthraquinone (94% pure ) in 410 g of 96% strength H2SO4 at 100° C. until the leuco compound has virtually completely disappeared. Excess chlorine and hydrogen chloride are blown out with air. The mixture is then allowed to cool down to room temperature while introducing 48.0 g of 1-aminoanthraquinone and the solution is then added dropwise to 410 g of water. 95.0 g of potassium peroxodisulphate are introduced in portions at 40°-50° C. within about 1 hour. The mixture is allowed to stir for approximately a further 30 minutes, the solid is filtered off with suction and washed with water until almost neutral. The filter cake is washed with 300 ml of 10% strength NaHSO3 solution and then with water and dried at 100° C. 102.3 g of 4,4'-diamino-1,1'-dianthrimide (79% pure), corresponding to 87% of theory, are obtained.

후처리

  1. filtrationthe solid is filtered off with suction
  2. washwashed with water until almost neutral
  3. washThe filter cake is washed with 300 ml of 10% strength NaHSO3 solution
  4. dry with materialwith water and dried at 100° C

출처 및 근거

ORD 기록
ord-4e7554c787d84b50a544ab83e5107ff3
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04452742

연결된 노트

불러오는 중…