1,2-Dichloroethane → N-(1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methyl-1-oxobutan-2-yl)-2-phenylacetamide

HRID 1820163노트

반응식

HRID 1820163 반응식
C1C=CC2N(O)N=NC=2C=1.[C:11]1([CH2:17][C:18]([OH:20])=O)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(Cl)CCl.Cl.[NH2:26][CH:27]([CH:43]([CH3:45])[CH3:44])[C:28]([N:30]1[CH2:35][CH2:34][CH:33]([C:36]2[CH:41]=[CH:40][C:39]([Cl:42])=[CH:38][CH:37]=2)[CH2:32][CH2:31]1)=[O:29]>CN(C=O)C.CCN(C(C)C)C(C)C.CO>[Cl:42][C:39]1[CH:40]=[CH:41][C:36]([CH:33]2[CH2:32][CH2:31][N:30]([C:28](=[O:29])[CH:27]([NH:26][C:18](=[O:20])[CH2:17][C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH:43]([CH3:45])[CH3:44])[CH2:35][CH2:34]2)=[CH:37][CH:38]=1

참가 물질

8

반응물 4

HCID 111,2-DichloroethaneHCID 999Phenylacetic AcidHCID 757711-HydroxybenzotriazoleHCID 672994912-Amino-1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methylbutan-1-one hydrochloride

생성물 1

HCID 24758856N-(1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methyl-1-oxobutan-2-yl)-2-phenylacetamide

시약·촉매·용매 3

HCID 887Methanol용매HCID 6228Dimethylformamide용매2회HCID 81531Diisopropylethylamine용매

실험 절차

A reaction tube was charged with HOBt (10 mg), phenylacetic acid (12 mg) and EDC (14 mg) in DMF (0.7 mL). The resulting mixture was agitated at rt. for 15 min, and then a solution of 2-amino-1-(4-(4-chlorophenyl)piperidin-1-yl)-3-methylbutan-1-one hydrochloride (20 mg) in DIEA (50 μL) and DMF (250 μL) was added and the resulting mixture was shaken overnight at rt. At the conclusion of this period, the resulting solution was diluted with MeOH and purified by preparative LC-MS to provide Example 9. MS found: (M+H)+=414.

후처리

  1. stirringthe resulting mixture was shaken overnight at rt
  2. custompurified by preparative LC-MS
  3. customto provide Example 9

출처 및 근거

ORD 기록
ord-59b3d913929847189f1a3af549b9fa13
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601844B2

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