4-Methylmorpholine → N-[2-(4-Amino-phenyl)-1-phenyl-ethyl]-2,2-diphenyl-acetamide

HRID 1886122

反応式

HRID 1886122 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH:9]([NH2:16])[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.[C:17]1([CH:23]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:24](O)=[O:25])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C1C=CC2N(O)N=NC=2C=1.CN1CCOCC1.CCN=C=NCCCN(C)C.Cl>CN(C)C=O>[C:10]1([CH:9]([NH:16][C:24](=[O:25])[CH:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:8][C:5]2[CH:4]=[CH:3][C:2]([NH2:1])=[CH:7][CH:6]=2)[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

参加物

7

反応物 5

HCID 79724-MethylmorpholineHCID 8333Diphenylacetic AcidHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 100590432-(4-Aminophenyl)-1-phenylethylamine

生成物 1

HCID 9953161N-[2-(4-Amino-phenyl)-1-phenyl-ethyl]-2,2-diphenyl-acetamide収率 88.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-(4-aminophenyl)-1-phenylethylamine (0.40 g, 1.9 mMol) and diphenylacetic acid (0.40 g, 1.9 mMol) were dissolved in dimethylformamide (DMF) (4 mL) at room temperature. To this was added HOBT (0.26 g, 1.9 mMol), NMM (0.19 g, 1.9 mMol) and EDCl (0.36 g) and the mixture was stirred at room temperature for 18 hours. The DMF was removed under vacuum and the oily residue was taken up in 100 mL ethyl acetate. The ethyl acetate was washed with saturated sodium bicarbonate and with brine, dried over magnesium sulfate, and evaporated to give 0.683 grams of a semi-solid. This was purified on 30 grams of flash-grade silica gel eluting with 100% dichloromethane to give 0.512 grams of the title compound, m.p. 161°-163° C.

後処理

  1. customThe DMF was removed under vacuum
  2. washThe ethyl acetate was washed with saturated sodium bicarbonate and with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-9b6f8594e30d4da2952ee3f3515cec3c
出典データセット
uspto-grants-1992_09
特許番号
US05149709

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