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Sodium hydride → HCID 66976191、化合物

HRID 1022632
ノート
印刷プレビュー

反応式

HRID 1022632 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1.[Br-].[Li+].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([C@@H:19]2[O:25][CH2:24][CH2:23][N:22]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:21][C@H:20]2[CH2:33]OS(C)(=O)=O)=[CH:15][C:14]=1[F:39]>COCCOC.CN(C=O)C.O>[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([C@@H:19]2[O:25][CH2:24][CH2:23][N:22]([C:26]([O:28][C:29]([CH3:31])([CH3:30])[CH3:32])=[O:27])[CH2:21][C@H:20]2[CH2:33][N:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]2=[O:3])=[CH:15][C:14]=1[F:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 82050Lithium BromideHCID 86663855tert-butyl (6S,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methylsulfonyl)oxy]methyl}-1,4-oxazepane-4-carboxylateHCID 178516071HCID 178516071、化合物

生成物 1

HCID 66976191HCID 66976191、化合物収率 81%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

60% Sodium hydride (45.3 mg, 1.13 mmol) was added to a mixed solution of 2-hydroxypyridine (86 mg, 0.91 mmol) in 1,2-dimethoxyethane (2 ml) and DMF (1 mL) at room temperature. After stirring at room temperature for 5 min, lithium bromide (131 mg, 1.51 mmol) was added at room temperature. After stirring for 10 min, to the reaction mixture was added a solution of tert-butyl (6S,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methylsulfonyl)oxy]methyl}-1,4-oxazepane-4-carboxylate (331 mg, 0.76 mmol) in 1,2-dimethoxyethane (2 mL). The reaction mixture was stirred at 80° C. overnight. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (267 mg, 0.611 mmol, 81%).

後処理

  1. stirringAfter stirring for 10 min, to the reaction mixture
  2. stirringThe reaction mixture was stirred at 80° C. overnight
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-0180fd37d59f4a38aa8a0244fed8b23b
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722662B2

反応ノート

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