Hydrochloric Acid → 2,6-Bis(4-methoxybenzoyl)naphthalene

HRID 893779

반응식

HRID 893779 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][C:7]([C:11](Cl)=[O:12])=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:14](Cl)=[O:15].[C:17]1([O:23][CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>[N+](C1C=CC=CC=1)([O-])=O.CN1CCCC1=O.O>[CH3:24][O:23][C:17]1[CH:22]=[CH:21][C:20]([C:14]([C:2]2[CH:3]=[CH:4][C:5]3[C:10](=[CH:9][CH:8]=[C:7]([C:11](=[O:12])[C:20]4[CH:21]=[CH:22][C:17]([O:23][CH3:24])=[CH:18][CH:19]=4)[CH:6]=3)[CH:1]=2)=[O:15])=[CH:19][CH:18]=1

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 7519AnisoleHCID 34855962,6-Naphthalenedicarbonyl dichlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 198911242,6-Bis(4-methoxybenzoyl)naphthalene

시약·촉매·용매 3

HCID 962Water용매HCID 7416Nitrobenzene용매HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

A stirred reactor comprising a 750 ml sulfonation flask, thermometer, condenser and nitrogen inlet is charged with 25.3 g (0.1 mol) of naphthalene-2,6-dicarbonyl dichloride and 32.4 g (0.2 mol) of anisole in 200 ml of nitrobenzene and, with stirring, 26.6 g (0.2 mol) of aluminium chloride are added over 15 minutes at 12°-18° C. The reaction mixture is thereafter allowed to react for 90 minutes at 40° C., then cooled to room temperature and thoroughly mixed with 1.5 liters of water containing HCl. The resultant suspension is diluted with 1.2 liters of N-methylpyrrolidone, and the mixture is heated to 130° C. The clear solution so obtained is cooled and the crystallised product is isolated by filtration. The filter residue is vacuum dried at 130° C., giving 25.9 g (65.4% of theory) of the desired product, which melts at 251° C.

후처리

  1. customA stirred reactor comprising
  2. customto react for 90 minutes at 40° C.
  3. temperaturethe mixture is heated to 130° C
  4. customThe clear solution so obtained
  5. temperatureis cooled
  6. customthe crystallised product is isolated by filtration
  7. customdried at 130° C.

출처 및 근거

ORD 기록
ord-40084545ddf24c55ab86285f440d97f2
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05126427

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