Acetic Acid → HCID 59264607, 화합물

HRID 1855628노트

반응식

HRID 1855628 반응식
[CH3:1][C:2]([N:9]1[CH2:14][CH2:13][C:12](=O)[CH2:11][CH2:10]1)([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].Cl.[F:17][C:18]([F:35])([F:34])[O:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2[CH:31]=[CH:30][C:29]([CH2:32][NH2:33])=[CH:28][CH:27]=2)=[CH:22][CH:21]=1.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>ClCCCl>[CH3:1][C:2]([N:9]1[CH2:14][CH2:13][CH:12]([NH:33][CH2:32][C:29]2[CH:30]=[CH:31][C:26]([C:23]3[CH:24]=[CH:25][C:20]([O:19][C:18]([F:17])([F:34])[F:35])=[CH:21][CH:22]=3)=[CH:27][CH:28]=2)[CH2:11][CH2:10]1)([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 229284574-(4-trifluoromethoxyphenyl)benzylamine HydrochlorideHCID 59264612Ethyl 2-methyl-2-(4-oxo-1-piperidinyl)propanoate

생성물 1

HCID 59264607HCID 59264607, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

A mixture of ethyl 2-methyl-2-(4-oxo-1-piperidinyl)propanoate (Int. A4) (1.09 g, 1.2 equiv), ({4′-[(trifluoromethyl)oxy]-4-biphenylyl}methyl)amine hydrochloride (Int. A2) (1.28 g, 1.0 equiv), DCE (21 ml) and acetic acid (0.27 ml, 1.1 equiv) was stirred at room temperature under nitrogen. Sodium triacetoxyborohydride (1.42 g, 1.5 equiv) was added and stirring continued for 3 hours. Aqueous sodium carbonate (2M solution, excess) was added and stirred for 45 min, then the mixture was partitioned with a mixture of diethyl ether/THF and water. The organic extracts were backwashed with water and brine, and dried over sodium sulfate and evaporated in vacuo. The desired product was obtained as a light yellow solid (2.14 g) which was used without further purification.

후처리

  1. stirringstirring
  2. stirringstirred for 45 min
  3. customthe mixture was partitioned with a mixture of diethyl ether/THF and water
  4. dry with materialdried over sodium sulfate
  5. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-92c5d1387c114058a42e03f7a11c9464
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962633B2

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