Hydrochloric Acid → HCID 58313095, 화합물

HRID 1748887노트

반응식

HRID 1748887 반응식
[C:1]([N:4]1[C:8]2([CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH:5]1[C:14]([O:16]CC)=[O:15])(=[O:3])[CH3:2].O.[OH-].[Li+].Cl>C1COCC1.O.CO>[C:1]([N:4]1[C:8]2([CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)[CH2:7][CH2:6][CH:5]1[C:14]([OH:16])=[O:15])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 58313107Ethyl 1-acetyl-8-oxa-1-azaspiro[4.5]decane-2-carboxylate

생성물 1

HCID 58313095HCID 58313095, 화합물수율 102.2%

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

실험 절차

To a solution of ethyl 1-acetyl-8-oxa-1-azaspiro[4.5]decane-2-carboxylate (170) (93 mg, 0.34 mmol) in THF/water/methanol (1.1 mL/0.6 mL/0.6 mL) was added lithium hydroxide monohydrate (29 mg, 0.69 mmol) and the reaction stirred at room temperature for 3 h. The reaction is treated with 1N HCl (0.7 mL) and partitioned between EtOAc and 0.1 N HCl, the aqueous layer was extracted twice with EtOAc, the combined organic layers were dried over MgSO4 and concentrated in vacuo to afford the title compound as a white solid (79 mg, 95% yield).

후처리

  1. custompartitioned between EtOAc and 0.1 N HCl
  2. extractionthe aqueous layer was extracted twice with EtOAc
  3. dry with materialthe combined organic layers were dried over MgSO4
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7636e9c6ff8244c2bcef6f6296895598
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150587B2

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