Nabumetone → Nabumetone 2,3-naphthalenediol

HRID 271035

反応式

HRID 271035 の反応式
[CH3:1][C:2]([CH2:4][CH2:5][C:6]1[CH:7]=[CH:8][C:9]2[CH:10]=[C:11]([O:16][CH3:17])[CH:12]=[CH:13][C:14]=2[CH:15]=1)=[O:3].[CH:18]1[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[C:20]([OH:28])[C:19]=1[OH:29]>[N+](C)([O-])=O>[CH:21]1[C:22]2[C:27](=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH:18]=[C:19]([OH:29])[C:20]=1[OH:28].[CH3:1][C:2]([CH2:4][CH2:5][C:6]1[CH:7]=[CH:8][C:9]2[CH:10]=[C:11]([O:16][CH3:17])[CH:12]=[CH:13][C:14]=2[CH:15]=1)=[O:3].[CH:13]1[C:14]2[C:9](=[CH:8][CH:7]=[CH:6][CH:15]=2)[CH:10]=[C:11]([OH:16])[C:12]=1[OH:28]

参加物

5

反応物 2

HCID 4409Nabumetone2 回HCID 70912,3-Dihydroxynaphthalene

生成物 2

HCID 70912,3-DihydroxynaphthaleneHCID 67107975Nabumetone 2,3-naphthalenediol収率 68%

試薬・触媒・溶媒 1

HCID 6375Nitromethane溶媒

実験手順

As a demonstrative example, a cocrystal comprising a neutral API is described in this example. Cocrystals of nabumetone (a neutral API) and 2,3-naphthalenediol were prepared as follows. A 4.01 g sample of 2,3-naphthalenediol and 5.7 g of nabumetone were dissolved in 50 mL of nitromethane with heating. A solid was formed as the solution cooled and was allowed to stand overnight. The solid was filtered from the remaining solvent and dried in the air to yield 6.61 g (68%) of nabumetone:2,3-naphthalenediol (1:1) cocrystal.

後処理

  1. temperaturewith heating
  2. customA solid was formed as the solution
  3. temperaturecooled
  4. filtrationThe solid was filtered from the remaining solvent
  5. customdried in the air

出典と根拠

ORDレコード
ord-f4aa8ea5a5884b2695c8e9085aab7d64
出典データセット
uspto-grants-2008_11
特許番号
US07452555B2

関連ノート

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