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HCID 11300027、化合物 → 1-(4-Benzyl-morpholin-2-yl)-2-methyl-propan-1-ol

HRID 131190
ノート
印刷プレビュー

反応式

HRID 131190 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH:14]([OH:18])[CH:15]([CH3:17])[CH3:16])[C:9]1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>O1CCCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH:14]([OH:18])[CH:15]([CH3:16])[CH3:17])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=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

3

反応物 1

HCID 11300027HCID 11300027、化合物

生成物 1

HCID 597321971-(4-Benzyl-morpholin-2-yl)-2-methyl-propan-1-ol収率 97%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

To a stirred solution of 53 (1.97 g, 7.47 mmol) in tetrahydrofuran (50 ml) at room temperature under nitrogen was added borane-tetrahydrofuran complex (30 ml of a 1M solution, ca 4 eq.). The reaction was heated to 60° C. and followed by TLC-analysis. When all starting material had been consumed a few drops of methanol were added followed by a similar amount of 1N hydrochloric acid and heating was continued for another hour. Organic solvents were removed in vacuo and the remaining solution was poured onto 1M potassium carbonate solution (30 ml), extracted with diethyl ether. The organic layers were dried over magnesium sulphate and purified by column chromatography (gradient from 15% ethyl acetate in hexane [v/v]) gave 54 (1.8 g, 97%). MW 249.36; C15H23NO2; LCMS (6 min method): m/z 250 [M+H]+; RT=0.838.

後処理

  1. customWhen all starting material had been consumed a few drops of methanol
  2. additionwere added
  3. temperatureheating
  4. waitwas continued for another hour
  5. customOrganic solvents were removed in vacuo
  6. additionthe remaining solution was poured onto 1M potassium carbonate solution (30 ml)
  7. extractionextracted with diethyl ether
  8. dry with materialThe organic layers were dried over magnesium sulphate
  9. custompurified by column chromatography (gradient from 15% ethyl acetate in hexane [v/v])

出典と根拠

ORDレコード
ord-778c50090c0341a3ad706c8e713d3e39
出典データセット
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07384941B2

反応ノート

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