Lithium Hydroxide → 880466-44-4

HRID 917316ノート

反応式

HRID 917316 の反応式
[OH-].[Li+].C([O:5][C:6]([CH:8]1[CH2:13][CH2:12][CH:11]([C:14]2[CH:15]=[C:16]3[C:21](=[C:22]([C:24]4[CH:29]=[CH:28][CH:27]=[C:26]([F:30])[CH:25]=4)[N:23]=2)[N:20]=[CH:19][CH:18]=[CH:17]3)[CH2:10][CH2:9]1)=[O:7])C>C1COCC1.CO>[F:30][C:26]1[CH:25]=[C:24]([C:22]2[N:23]=[C:14]([CH:11]3[CH2:10][CH2:9][CH:8]([C:6]([OH:7])=[O:5])[CH2:13][CH2:12]3)[CH:15]=[C:16]3[C:21]=2[N:20]=[CH:19][CH:18]=[CH:17]3)[CH:29]=[CH:28][CH:27]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 69399171HCID 69399171、化合物

生成物 1

HCID 9924539880466-44-4

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

Lithium hydroxide (1M (aq), 24.3 ml, 24.3 mmol) is added to a solution of 4-[8-(3-fluorophenyl)-[1,7]naphthyridin-6-yl]-cyclohexanecarboxylic acid ethyl ester (4.60 g, 12.14 mmol) in THF/methanol (40 ml:20 ml) and stirred at room temperature overnight. The organic solvents are removed by evaporation, then the aqueous residue diluted with water and basified to pH9 with 1M KOH. The aqueous layer is then washed with ethyl acetate (3×). The aqueous layer is acidified to pH 4 with 1M HCl to give a white precipitate, which is extracted into ethyl acetate. The ethyl acetate layer is then dried over sodium sulfate, filtered and concentrated to yield the desired product as a yellow foam. Further trituration with 1M HCl yields the product as a pale yellow powder (2.153 g). MS (AP+) 350.6

後処理

  1. customThe organic solvents are removed by evaporation
  2. additionthe aqueous residue diluted with water and basified to pH9 with 1M KOH
  3. washThe aqueous layer is then washed with ethyl acetate (3×)
  4. customto give a white precipitate, which
  5. extractionis extracted into ethyl acetate
  6. dry with materialThe ethyl acetate layer is then dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-8ff623813018435ead8a9538cff71815
出典データセット
uspto-grants-2007_09
特許番号
US07273875B2

反応ノート

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