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Sodium hydride → 3-Methoxy-N-(2-methoxyphenyl)-N-(2-tetrahydropyranyloxyethyl)benzamide

HRID 2462
ノート
印刷プレビュー

反応式

HRID 2462 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15][CH3:16])=[O:7].[H-].[Na+].[O:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[O:28][CH2:29][CH2:30]Br>CN(C=O)C>[O:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH:23]1[O:28][CH2:29][CH2:30][N:8]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15][CH3:16])[C:6](=[O:7])[C:5]1[CH:17]=[CH:18][CH:19]=[C:3]([O:2][CH3:1])[CH:4]=1
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 24758Sodium hydrideHCID 866212-(2-Bromoethoxy)tetrahydro-2H-pyranHCID 9028663-methoxy-N-(2-methoxyphenyl)benzamide

生成物 1

HCID 539260843-Methoxy-N-(2-methoxyphenyl)-N-(2-tetrahydropyranyloxyethyl)benzamide収率 67%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In an atmosphere of argon, 3-methoxy-N-(2-methoxyphenyl) benzamide (500 mg, 1.94 mmol) was dissolved in DMF (10 ml) to which was subsequently added sodium hydride (85 mg, 60%, 2.13 mmol) at room temperature, followed by 20 minutes of stirring. After additional 5 minutes of stirring under an ultrasonic irradiation condition at the same temperature, to this was added 2-tetrahydropyranyloxyethyl bromide (446 mg, 2.13 mmol) at room temperature. After 1 hour of stirring at room temperature and subsequent stirring at 70° C. for 6 hours, DMF was removed by evaporation, and the resulting residue was mixed with water (20 ml), extracted with ether and then washed with water and saturated brine. The resulting organic layer was dried on anhydrous magnesium sulfate, the solvent was removed by evaporation and then the resulting orange oily residue was purified by subjecting it to a silica gel column chromatography (ether:hexane=2:1) to obtain 501 mg (67.0%) of the title compound in the form of yellow oil.

後処理

  1. customat room temperature
  2. stirringAfter additional 5 minutes of stirring under an ultrasonic irradiation condition at the same temperature
  3. stirringAfter 1 hour of stirring at room temperature
  4. stirringsubsequent stirring at 70° C. for 6 hours
  5. customDMF was removed by evaporation
  6. additionthe resulting residue was mixed with water (20 ml)
  7. extractionextracted with ether
  8. washwashed with water and saturated brine
  9. dry with materialThe resulting organic layer was dried on anhydrous magnesium sulfate
  10. customthe solvent was removed by evaporation
  11. customthe resulting orange oily residue was purified

出典と根拠

ORDレコード
ord-3ded3b8d2ed540a4b76f3f398d06c312
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05728835

反応ノート

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