Tetrafluoroboric acid → 4-Hydroxy-1,8-naphthalenedicarboxylic anhydride

HRID 278978

반응식

HRID 278978 반응식
[CH:1]1[CH:10]=[C:9]2[C:11]([O:13][C:14](=[O:15])[C:7]3=[C:8]2[C:3](=[C:4](N)[CH:5]=[CH:6]3)[CH:2]=1)=[O:12].N([O-])=[O:18].[Na+].F[B-](F)(F)F.[H+]>S(=O)(=O)(O)O.O>[CH:1]1[CH:10]=[C:9]2[C:11]([O:13][C:14](=[O:15])[C:7]3=[C:8]2[C:3](=[C:4]([OH:18])[CH:5]=[CH:6]3)[CH:2]=1)=[O:12]

참가 물질

6

반응물 3

HCID 28118Tetrafluoroboric acidHCID 809904-Aminonaphthalene-1,8-dicarboxylic anhydrideHCID 23668193Sodium Nitrite

생성물 1

HCID 59994974-Hydroxy-1,8-naphthalenedicarboxylic anhydride수율 61.6%

시약·촉매·용매 2

HCID 962Water용매2회HCID 1118Sulfuric Acid용매2회

실험 절차

To a solution of 1.0 g (4.7 mmol) of 4-amino-1,8-naphthalic anhydride in 5 mL concentrated sulfuric acid at 0° C. to 5° C. was added 1.0 g (14.5 mmol) of sodium nitrite, and then 0.5 mL of water. The reaction was stirred for 30 minutes at 0° C. to 5° C., followed by addition of 5 mL (38 mmol) of 48% aqueous fluoroboric acid, with stirring for 30 minutes. The mixture was poured into ice water. The precipitate was isolated, suspended in a solution of 10 mL concentrated sulfuric acid in 50 mL water, refluxed for 3 hours, and again poured onto ice. The precipitate was isolated, washed with water, and dried to yield 620 mg of the title compound.

후처리

  1. stirringwith stirring for 30 minutes
  2. customThe precipitate was isolated
  3. temperaturerefluxed for 3 hours
  4. additionagain poured onto ice
  5. customThe precipitate was isolated
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-8aecf3b11c6d4a569e58523b7a85b81b
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06362181B1

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