Phenol → 14H-benz[4,5]isoquino[2,1-a]perimidin-14-one

HRID 260890

반응식

HRID 260890 반응식
C1(O)C=CC=CC=1.[NH2:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][C:17]=2[NH2:19])[CH:12]=[CH:11][CH:10]=1.[CH:20]1[CH:25]=[C:24]2[C:26](O[C:29]([C:31]3=[CH:32][CH:33]=[CH:34][C:22](=[C:23]23)[CH:21]=1)=O)=[O:27]>CO>[CH:16]1[C:17]2=[C:18]3[C:13]([CH:12]=[CH:11][CH:10]=[C:9]3[N:8]=[C:29]3[C:31]4[CH:32]=[CH:33][CH:34]=[C:22]5[CH:21]=[CH:20][CH:25]=[C:24]([C:23]=45)[C:26](=[O:27])[N:19]32)=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 996PhenolHCID 6693Naphthalic anhydrideHCID 680671,8-Diaminonaphthalene

생성물 1

HCID 8127114H-benz[4,5]isoquino[2,1-a]perimidin-14-one

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
150 °C

실험 절차

250 g of phenol are melted at about 60° C. 47.4 g of 1,8-diaminonaphthalene and 59.4 g of 1,8-naphthalic acid anhydride are introduced, while passing over nitrogen, and the mixture is heated to 150° C. in the course of 1 hour and kept at this temperature for 2 hours. The reaction mixture is cooled to 80° C., 120 ml of methanol are added at a temperature of 80° to 65° C. in the course of 30 minutes, and the mixture is cooled to room temperature and filtered with suction. After the residue has been washed with 240 ml of methanol and dried at 150° C., 88.8 g of the stated dyestuff are obtained in a very good quality.

후처리

  1. temperatureThe reaction mixture is cooled to 80° C.
  2. temperaturethe mixture is cooled to room temperature
  3. filtrationfiltered with suction
  4. washAfter the residue has been washed with 240 ml of methanol
  5. customdried at 150° C.
  6. custom88.8 g of the stated dyestuff are obtained in a very good quality

출처 및 근거

ORD 기록
ord-222415fb05e64196981cfd7fb30e071f
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05530130

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