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

HRID 1820296
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HRID 1820296 반응식
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
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b05445d2cc234bd69232bc0538b13fa0
출처 데이터셋
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07601843B2

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