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Sodium hydride → Carbamic acid, N-[[4-[(4,6-dichloro-2-pyrimidinyl)oxy]phenyl]methyl]-, 1,1-dimethylethyl ester

HRID 1403129
ノート
印刷プレビュー

反応式

HRID 1403129 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:18]=[CH:17][C:7]([CH2:8][NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:6][CH:5]=1.[Cl:19][C:20]1[CH:25]=[C:24]([Cl:26])[N:23]=[C:22](S(C)(=O)=O)[N:21]=1.[Cl-].[NH4+]>COCCOC>[C:12]([O:11][C:10](=[O:16])[NH:9][CH2:8][C:7]1[CH:17]=[CH:18][C:4]([O:3][C:22]2[N:23]=[C:24]([Cl:26])[CH:25]=[C:20]([Cl:19])[N:21]=2)=[CH:5][CH:6]=1)([CH3:14])([CH3:15])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 2396854,6-Dichloro-2-(methylsulfonyl)pyrimidineHCID 11085418tert-butyl 4-hydroxybenzylcarbamate

生成物 1

HCID 101043327Carbamic acid, N-[[4-[(4,6-dichloro-2-pyrimidinyl)oxy]phenyl]methyl]-, 1,1-dimethylethyl ester

試薬・触媒・溶媒 1

HCID 8071
1,2-Dimethoxyethane
溶媒

実験手順

60% Sodium hydride (394 mg) was suspended in 1,2-dimethoxyethane (20 mL), and tert-butyl 4-hydroxybenzylcarbamate (1 g) and 15-crown-5-ether (1.09 g) were added thereto, followed by stirring at room temperature for 30 minutes. 4,6-Dichloro-2-(methylsulfonyl)pyrimidine was added thereto, followed by stirring at 80° C. overnight. The reaction solution was cooled to room temperature and then an aqueous ammonium chloride solution (50 mL) was added thereto, followed by extraction with ethyl acetate. The extracts were washed with water and saturated brine, and the organic layer was dried over anhydrous magnesium sulfate. The desiccant was removed by filtration and the solvent was evaporated under reduced pressure. The residue was purified using silica gel column chromatography (hexane:ethyl acetate=95:5-85:15) to obtain tert-butyl{-4-[(4,6-dichloropyrimidin-2-yl)oxy]benzyl}carbamate (762 mg).

後処理

  1. stirringby stirring at 80° C. overnight
  2. temperatureThe reaction solution was cooled to room temperature
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe extracts were washed with water and saturated brine
  5. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  6. customThe desiccant was removed by filtration
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified

出典と根拠

ORDレコード
ord-872eda49922a4c1d933d6d5a435ca04b
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912180B2

反応ノート

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