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

HRID 1016093ノート

反応式

HRID 1016093 の反応式
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

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒2 回HCID 81531Diisopropylethylamine溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-389a42b0707243d6bef34c724bbbacf7
出典データセット
uspto-grants-2011_07
特許番号
US07985861B2

反応ノート

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