Sodium Hydroxide → HCID 11212544、化合物

HRID 349737

反応式

HRID 349737 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.[C:16]([N:23]1[CH2:28][CH2:27][C:26](=O)[CH2:25][CH2:24]1)([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17].[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].[OH-].[Na+]>ClCCCl.C(OCC)C.C(O)(=O)C>[C:19]([O:18][C:16]([N:23]1[CH2:28][CH2:27][CH:26]([N:9]2[CH2:10][CH2:11][CH:6]([O:5][C:4]3[CH:12]=[CH:13][C:14]([Cl:15])=[C:2]([Cl:1])[CH:3]=3)[CH2:7][CH2:8]2)[CH2:25][CH2:24]1)=[O:17])([CH3:22])([CH3:20])[CH3:21]

参加物

8

反応物 4

HCID 14798Sodium HydroxideHCID 735900tert-Butyl 4-oxopiperidine-1-carboxylateHCID 37320424-(3,4-Dichlorophenoxy)piperidineHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 11212544HCID 11212544、化合物

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 176Acetic Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

4-(3,4-Dichlorophenoxy)piperidine (1.5 g) was dissolved in 1,2-dichloroethane (21 ml). 1-Boc-4-piperidone was added (1.21 g) followed by NaBH(OAc)3 (1.81 g) and acetic acid (0.37 g). After 18 hours at room temperature aqueous NaOH (1M) solution and diethyl ether were added. The product was extracted with diethyl ether, the combined organic extracts dried with MgSO4 and concentrated. Purification by silica chromatography (dichloromethane:methanol 92:8) gave the sub-title product (1.97 g).

後処理

  1. extractionThe product was extracted with diethyl ether
  2. dry with materialthe combined organic extracts dried with MgSO4
  3. concentrationconcentrated
  4. customPurification by silica chromatography (dichloromethane:methanol 92:8)

出典と根拠

ORDレコード
ord-b56cf4608c2f41898801741083f5e15f
出典データセット
uspto-grants-2007_02
特許番号
US07179922B2

関連ノート

読み込み中…