1,4,5,8-Naphthalenetetracarboxylic acid → 1,3-Dioxo-1H,3H-naphtho(1,8-cd)pyran-6,7-dicarboxylic acid

HRID 1656857

반응식

HRID 1656857 반응식
[C:1]1([C:20]([OH:22])=[O:21])[C:10]2[C:9]([C:11]([OH:13])=[O:12])=[CH:8][CH:7]=[C:6]([C:14]([OH:16])=[O:15])[C:5]=2[C:4]([C:17]([OH:19])=O)=[CH:3][CH:2]=1.[Na][Na]>O.C1C(C(N)=O)=CN(C2OC(COP(OP(OCC3OC(N4C5N=CN=C(N)C=5N=C4)C(OP([O-])([O-])=O)C3O)([O-])=O)([O-])=O)C(O)C2O)C=C1.[Na+].[Na+].[Na+].[Na+]>[C:6]12[C:14](=[O:16])[O:15][C:17](=[O:19])[C:4]3[C:5]1=[C:10]([C:1]([C:20]([OH:22])=[O:21])=[CH:2][CH:3]=3)[C:9]([C:11]([OH:13])=[O:12])=[CH:8][CH:7]=2

참가 물질

5

반응물 2

HCID 314221,4,5,8-Naphthalenetetracarboxylic acid2회HCID 141233Disodium

생성물 1

HCID 1323361,3-Dioxo-1H,3H-naphtho(1,8-cd)pyran-6,7-dicarboxylic acid수율 97%

시약·촉매·용매 2

HCID 962Water용매HCID 12598259[2-adenin-9-yl-5-[[[[5-(3-carbamoyl-4H-pyridin-1-yl)-3,4-dihydroxy-tetrahydrofuran-2-yl]methoxy-oxido-phosphoryl]oxy-oxido-phosphoryl]oxymethyl]-4-hydroxy-tetrahydrofuran-3-yl] phosphate용매2회

실험 절차

After cooling to a temperature of 20° to 30° C., the suspension, which was present after the letting down, of the tetrasodium salt of naphthalene-1,4,5,8-tetracarboxylic acid (NTC) was worked up by a process analogous to that described in Example 3 c) , by a procedure in which the disodium salt of NTC was first formed by acidification to pH 4.8 to 4.5 and was isolated, this salt was then dissolved in water by conversion into the tetrasodium salt, insoluble impurities were separated off by filtration, and the 1,8-monoanhydride of NTC was then precipitated by acidification with hydrochloric acid and was isolated. 13.1 kg of naphthalene-1,4,5,8-tetracarboxylic acid 1,8-monoanhydride of 96% purity, corresponding to a yield of 97% of theory, were obtained.

후처리

  1. temperatureAfter cooling to a temperature of 20° to 30° C.
  2. customwas first formed by acidification to pH 4.8 to 4.5
  3. customwas isolated
  4. customwere separated off by filtration
  5. customthe 1,8-monoanhydride of NTC was then precipitated by acidification with hydrochloric acid
  6. customwas isolated

출처 및 근거

ORD 기록
ord-20723f5bb0344f3383d0149c69f6c215
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05254796

연결된 노트

불러오는 중…