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Ammonia → HCID 22013876、化合物

HRID 1532741
ノート
印刷プレビュー

反応式

HRID 1532741 の反応式
[C:1]([NH:4][CH:5]([CH2:11][C:12]1[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][C:21]2[N:22]=[C:23]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[O:24][C:25]=2[CH3:26])=[CH:14][CH:13]=1)[C:6](OCC)=[O:7])(=[O:3])[CH3:2].[NH3:33].[OH-].[Na+]>CO.O1CCCC1>[C:1]([NH:4][CH:5]([CH2:11][C:12]1[CH:13]=[CH:14][C:15]([O:18][CH2:19][CH2:20][C:21]2[N:22]=[C:23]([C:27]3[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=3)[O:24][C:25]=2[CH3:26])=[CH:16][CH:17]=1)[C:6]([NH2:33])=[O:7])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 222AmmoniaHCID 14798Sodium HydroxideHCID 22013867HCID 22013867、化合物

生成物 1

HCID 22013876HCID 22013876、化合物収率 36%

試薬・触媒・溶媒 1

HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

Ethyl 2-acetylamino-3-[4-[2-(5-methyl-2-phenyl-4-oxazolyl)ethoxy]phenyl]propionate (1.63 g, 3.73 mmol) obtained in Example 33 was dissolved in methanol-tetrahydrofuran (1:1, 50 ml). 28% Aqueous ammonia (20 ml) was added and the mixture was stirred at room temperature for 2 days. Thereto was added 1N aqueous sodium hydroxide solution (30 ml) and the mixture was stirred for 1 hr. The solvent was evaporated under reduced pressure and the obtained residue was partitioned between tetrahydrofuran-ethyl acetate (1:1, 100 ml) and water (50 ml). The organic layer was washed with saturated brine (50 ml), dried over magnesium sulfate and concentrated under reduced pressure. The residue (1.00 g) was washed with hot methanol to give the title compound (560 mg, yield 36%) as a white solid.

後処理

  1. stirringthe mixture was stirred for 1 hr
  2. customThe solvent was evaporated under reduced pressure
  3. customthe obtained residue was partitioned between tetrahydrofuran-ethyl acetate (1:1, 100 ml) and water (50 ml)
  4. washThe organic layer was washed with saturated brine (50 ml)
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. washThe residue (1.00 g) was washed with hot methanol

出典と根拠

ORDレコード
ord-919bbd78ee9c496db74036e055e27299
出典データセット
uspto-grants-2001_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06204277B1

反応ノート

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