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

HRID 1656857

反応式

HRID 1656857 の反応式
[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

参加物

5

反応物 2

HCID 314221,4,5,8-Naphthalenetetracarboxylic acid2 回HCID 141233Disodium

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 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] phosphate溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-20723f5bb0344f3383d0149c69f6c215
出典データセット
uspto-grants-1993_10
特許番号
US05254796

関連ノート

読み込み中…