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Hydrochloric Acid → 4-[2-[1-(2-Hydroxyethyl)cyclohexyl]ethyl]morpholine

HRID 1820296
ノート
印刷プレビュー

反応式

HRID 1820296 の反応式
Cl.[O:2]([CH2:20][CH2:21][C:22]1([CH2:28][CH2:29][N:30]2[CH2:35][CH2:34][O:33][CH2:32][CH2:31]2)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1)[Si](C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1>CO>[OH:2][CH2:20][CH2:21][C:22]1([CH2:28][CH2:29][N:30]2[CH2:31][CH2:32][O:33][CH2:34][CH2:35]2)[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 574278614-[2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl]morpholine

生成物 1

HCID 231098894-[2-[1-(2-Hydroxyethyl)cyclohexyl]ethyl]morpholine収率 94.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

After adding concentrated hydrochloric acid (0.5 mL, 6.0 mmol) to a solution of 4-[2-[1-[2-(tert-butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl]morpholine (1.31 g, ca. 1.97 mmol) in methanol (10 mL) at room temperature, the mixture was stirred for 4.5 hours. The reaction mixture was then concentrated under reduced pressure, 1N hydrochloric acid (10 mL) was added to the obtained residue, and extraction was performed with diethyl ether. After adding 5N aqueous sodium hydroxide to the aqueous layer to adjust the pH to 12, extraction was performed with diethyl ether. The organic layer was dried (anhydrous sodium sulfate) and then the solvent was distilled off under reduced pressure to obtain the title compound as a colorless oil (448 mg) (94% yield, 2 steps).

後処理

  1. concentrationThe reaction mixture was then concentrated under reduced pressure, 1N hydrochloric acid (10 mL)
  2. additionwas added to the obtained residue, and extraction
  3. additionAfter adding 5N aqueous sodium hydroxide to the aqueous layer
  4. extractionto 12, extraction
  5. dry with materialThe organic layer was dried (anhydrous sodium sulfate)
  6. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-b05445d2cc234bd69232bc0538b13fa0
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07601843B2

反応ノート

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