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Sodium Bicarbonate → 4-(4-Nitro-2-(trifluoromethyl)phenoxy)-1-(oxetan-3-yl)piperidine

HRID 633413
ノート
印刷プレビュー

反応式

HRID 633413 の反応式
[N+:1]([C:4]1[CH:16]=[CH:15][C:7]([O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[C:6]([C:17]([F:20])([F:19])[F:18])[CH:5]=1)([O-:3])=[O:2].[O:21]1[CH2:24][C:23](=O)[CH2:22]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C([O-])(O)=O.[Na+]>ClCCCl.C(Cl)Cl>[N+:1]([C:4]1[CH:16]=[CH:15][C:7]([O:8][CH:9]2[CH2:14][CH2:13][N:12]([CH:23]3[CH2:24][O:21][CH2:22]3)[CH2:11][CH2:10]2)=[C:6]([C:17]([F:20])([F:18])[F:19])[CH:5]=1)([O-:3])=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 150242543-OxetanoneHCID 207353814-(4-Nitro-2-(trifluoromethyl)phenoxy)piperidine

生成物 1

HCID 867045074-(4-Nitro-2-(trifluoromethyl)phenoxy)-1-(oxetan-3-yl)piperidine収率 77%

試薬・触媒・溶媒 2

HCID 11
1,2-Dichloroethane
溶媒
HCID 6344Dichloromethane溶媒

実験手順

A solution of 4-(4-nitro-2-(trifluoromethyl)phenoxy)piperidine (1.0 g, 1.0 eq, 3.5 mmol) and oxetan-3-one (0.35 g, 1.4 eq, 4.8 mmol) in 1,2-dichloroethane (50 mL) was stirred at room temperature for 30 minutes. Sodium triacetoxyborohydride (1.3 g, 1.8 eq, 6.2 mmol) was added in portions to the above solution and the heterogeneous mixture was stirred at room temperature overnight. The reaction mixture was diluted with CH2Cl2 (50 mL) and pardoned with aqueous saturated NaHCO3 solution (100 mL). The layers were separated and the organic layer was washed with brine solution (2×50 mL). The combined organic layers were dried over Na2SO4. Removal of the solvents and purification of the crude mixture by column chromatography on silica gel (ISCO System) using 20% MeOH in CH2Cl2/CH2Cl2 (gradient system from 0:1 to 1:9) as eluent gave the product in 77% yield.

後処理

  1. customThe layers were separated
  2. washthe organic layer was washed with brine solution (2×50 mL)
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. customRemoval of the solvents and purification of the crude mixture by column chromatography on silica gel (ISCO System)
  5. customgave the product in 77% yield

出典と根拠

ORDレコード
ord-2633f3fca6f54aec92bb7b414a9677b9
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09321763B2

反応ノート

読み込み中…

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