Tetraethyl 5,5'-(1,8-naphthyridine-2,7-diyl)diisophthalate → 5,5'-(1,8-Naphthyridine-2,7-diyl)diisophthalic acid

HRID 1484218ノート

反応式

HRID 1484218 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[CH:12]=[C:13]([C:22]([O:24]CC)=[O:23])[CH:14]=[C:15]([CH:21]=3)[C:16]([O:18]CC)=[O:17])[N:9]=2)[CH:4]=[CH:3][C:2]=1[C:27]1[CH:28]=[C:29]([C:38]([O:40]CC)=[O:39])[CH:30]=[C:31]([CH:37]=1)[C:32]([O:34]CC)=[O:33]>C1COCC1.CO.[OH-].[Na+]>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([C:11]3[CH:21]=[C:15]([C:16]([OH:18])=[O:17])[CH:14]=[C:13]([CH:12]=3)[C:22]([OH:24])=[O:23])[N:9]=2)[CH:4]=[CH:3][C:2]=1[C:27]1[CH:37]=[C:31]([C:32]([OH:34])=[O:33])[CH:30]=[C:29]([CH:28]=1)[C:38]([OH:40])=[O:39]

参加物

5

反応物 1

HCID 117940372Tetraethyl 5,5'-(1,8-naphthyridine-2,7-diyl)diisophthalate

生成物 1

HCID 706984375,5'-(1,8-Naphthyridine-2,7-diyl)diisophthalic acid

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

2.0 g of tetraethyl 5,5′-(1,8-naphthyridine-2,7-diyl)diisophthalate was dissolved in 60 mL of mixed solvent of THF and MeOH (v/v=1:1), 20 mL of 2N NaOH aqueous solution was added. The mixture was stirred at room temperature overnight. After the organic phase was removed, the aqueous phase was acidified with dilute hydrochloric acid to give white precipitate, which was filtered and washed with water several times. Yield: 1.5 g, 94%. 1H NMR (300 MHz, DMSO-d6): δ 8.44 (d, 2H), 8.62 (s, 2H), 8.68 (d, 2H), 9.10 (s, 4H).

後処理

  1. additionwas added
  2. customAfter the organic phase was removed
  3. customto give white precipitate, which
  4. filtrationwas filtered
  5. washwashed with water several times

出典と根拠

ORDレコード
ord-9af959f2d5604b48a87bb48424671ff9
出典データセット
uspto-grants-2016_08
特許番号
US09421514B2

反応ノート

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