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Sodium Hydroxide → 5-Benzyl-4,5,6,7-tetrahydro-furo[3,2-c]pyridine

HRID 2301102
ノート
印刷プレビュー

反応式

HRID 2301102 の反応式
Cl[CH2:2][CH2:3][N:4]([CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH2:5][C:6]1[CH:10]=[CH:9][O:8][CH:7]=1.CCCCCC.C([Li])CCC.[OH-].[Na+]>O1CCCC1>[CH2:11]([N:4]1[CH2:3][CH2:2][C:7]2[O:8][CH:9]=[CH:10][C:6]=2[CH2:5]1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
参加物反応条件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 14798Sodium HydroxideHCID 18377420N-benzyl-N-(3-furylmethyl)-2-chloroethylamineHCID 178418244HCID 178418244、化合物

生成物 1

HCID 183773045-Benzyl-4,5,6,7-tetrahydro-furo[3,2-c]pyridine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

2-(Benzyl-(3-furylmethyl)amino)ethanol (6.5 g, 28 mmol), triethylamine (5.9 ml, 42 mmol), 4-dimethylaminopyridine (250 mg, 2.1 mmol) and tosyl chloride (6.4 g, 34 mmol) were stirred at room temperature for 17 hours in dichloromethane (260 ml). The reaction solution was mixed with dichloromethane, washed with water and saturated brine and then dried with anhydrous magnesium sulfate. The solvent was removed by evaporation from the organic layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 5.4 g of crude 1-chloro-2-(benzyl-(3-furylmethyl)amino)ethane. The crude 1-chloro-2-(benzyl-(3-furylmethyl)amino)ethane (1.8 g) was dissolved in anhydrous tetrahydrofuran (35 ml) and cooled to 0° C. In an atmosphere of argon, n-butyl lithium hexane solution (14 mmol) was added thereto to carry out 2 hours of the reaction at room temperature. The reaction solution was mixed with 1 N sodium hydroxide aqueous solution, the reaction product was extracted with dichloromethane, and then the organic layer was washed with saturated brine and dried with anhydrous magnesium sulfate. The solvent was removed by evaporation from the organic layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 1.1 g (5.1 mmol, 73% in yield) of the title compound.

後処理

  1. customto carry out 2 hours of the reaction at room temperature
  2. extractionthe reaction product was extracted with dichloromethane
  3. washthe organic layer was washed with saturated brine
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was removed by evaporation from the organic layer under a reduced pressure
  6. customthe thus obtained material was separated
  7. custompurified by a silica gel column chromatography
  8. customto obtain

出典と根拠

ORDレコード
ord-74c4d472cf414d6990de5cfcdad30e7d
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06498251B1

反応ノート

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