1,2-Dichloroethane → HCID 131727750, 화합물

HRID 1912482노트

반응식

HRID 1912482 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[C:15]([NH:22][C@@H:23]1[CH2:28][CH2:27][CH2:26][C@H:25]([C:29](O)=[O:30])[CH2:24]1)([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16].C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:14][CH2:13][N:12]([C:29]([C@@H:25]3[CH2:26][CH2:27][CH2:28][C@H:23]([NH:22][C:15](=[O:16])[O:17][C:18]([CH3:20])([CH3:19])[CH3:21])[CH2:24]3)=[O:30])[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 936011-(3,4-Dichlorophenyl)piperazineHCID 2755995rel-(1R,3S)-3-[[(1,1-Dimethylethoxy)carbonyl]amino]cyclohexanecarboxylic acid

생성물 1

HCID 131727750HCID 131727750, 화합물수율 92.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of 4-(3,4-dichlorophenyl)piperazine (350 mg, 1.51 mmol), cis-3-(N-Boc-amino)cyclohexane carboxylic acid (368 mg, 1.51 mmol), HOBt (209 mg, 1.51 mmol) and EDC (291 mg, 1.51 mmol) was added dichloromethane followed by TEA (153 mg, 1.51 mmoL). Upon completion of addition, the resulting solution was allowed to stir overnight. At the conclusion of this period, the reaction mixture was concentrated and then purified via silica gel chromatography (20% to 50% EtOAc/hexanes) to provide the title compound (640 mg) as an oil.

후처리

  1. additionUpon completion of addition
  2. concentrationAt the conclusion of this period, the reaction mixture was concentrated
  3. custompurified via silica gel chromatography (20% to 50% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-926f7fd8f68e45df904f840434476a33
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609664B2

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