Acetic Acid → HCID 59264607、化合物

HRID 573481ノート

反応式

HRID 573481 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 59264607HCID 59264607、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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 contined 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.

後処理

  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

出典と根拠

ORDレコード
ord-6a249da4753145f6ade8ada9c016e1d3
出典データセット
uspto-grants-2015_05
特許番号
US09029383B2

反応ノート

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