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Hydrochloric Acid → 1-(2-Hydroxyethyl)piperazin-2-one

HRID 639991
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HRID 639991 반응식
[Si]([O:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13][C:12]1=[O:24])(C(C)(C)C)(C)C.Cl>O1CCOCC1>[OH:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][C:12]1=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 68638537Tert-butyl 4-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-3-oxopiperazine-1-carboxylate

생성물 1

HCID 132438661-(2-Hydroxyethyl)piperazin-2-one수율 57%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A mixture of tert-butyl 4-(2-{[tert-butyl(dimethyl)silyl]oxy}ethyl)-3-oxopiperazine-1-carboxylate (3.4 g, 9.50 mmol) and hydrogen chloride (15 ml of a 4M solution in 1,4-dioxane) in 1,4-dioxane (10 ml) was stirred at room temperature for 4 hour and then the mixture was evaporated. The residue was dissolved in a mixture of 5% methanol in dichloromethane (30 ml), basified with a 7N solution of ammonia in methanol and then filtered. The filtrate was evaporated and the residue was purified by silica gel chromatography eluting with 10% methanol in dichloromethane containing 0-5% 7M ammonia in methanol to give 1-(2-hydroxyethyl)piperazin-2-one (0.708 g, 57% yield) as a pale yellow oil.

후처리

  1. customthe mixture was evaporated
  2. dissolutionThe residue was dissolved in a mixture of 5% methanol in dichloromethane (30 ml)
  3. filtrationfiltered
  4. customThe filtrate was evaporated
  5. customthe residue was purified by silica gel chromatography
  6. washeluting with 10% methanol in dichloromethane containing 0-5% 7M ammonia in methanol

출처 및 근거

ORD 기록
ord-87449b1ef112498dad7f80abeec664e3
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691867B2

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