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Triethylamine → 1-Acryloyl-4-(2-((2',5',6-trichloro-4-methoxy-[1,1'-biphenyl]-3-yl)amino)acetyl)piperazine-2-carboxamide

HRID 588823
ノート
印刷プレビュー

反応式

HRID 588823 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[C:9]1[C:14]([Cl:15])=[CH:13][C:12]([O:16][CH3:17])=[C:11]([NH:18][CH2:19][C:20]([OH:22])=O)[CH:10]=1.CCN(CC)CC.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1.Cl.[C:53]([N:57]1[CH2:62][CH2:61][NH:60][CH2:59][CH:58]1[C:63]([NH2:65])=[O:64])(=[O:56])[CH:54]=[CH2:55]>CN(C=O)C>[C:53]([N:57]1[CH2:62][CH2:61][N:60]([C:20](=[O:22])[CH2:19][NH:18][C:11]2[CH:10]=[C:9]([C:3]3[CH:4]=[C:5]([Cl:8])[CH:6]=[CH:7][C:2]=3[Cl:1])[C:14]([Cl:15])=[CH:13][C:12]=2[O:16][CH3:17])[CH2:59][CH:58]1[C:63]([NH2:65])=[O:64])(=[O:56])[CH:54]=[CH2:55]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 90455762(2',5',6-Trichloro-4-methoxy-[1,1'-biphenyl]-3-yl)glycineHCID 904602351-Acryloylpiperazine-2-carboxamide hydrochloride

生成物 1

HCID 117610931
1-Acryloyl-4-(2-((2',5',6-trichloro-4-methoxy-[1,1'-biphenyl]-3-yl)amino)acetyl)piperazine-2-carboxamide
収率 3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

2-((2′,5′,6-Trichloro-4-methoxy-[1,1′-biphenyl]-3-yl)amino)acetic acid (231 mg, 0.641 mmol) and Et3N (592 mg, 2.564 mmol) in DMF (3 mL) at 0° C., EDCI.HCl (184 mg, 0.961 mmol) and HOBt (134 mg, 0.961 mmol) were added and the resulting mixture was stirred at 0° C. for 30 min. To this mixture, the above 1-acryloylpiperazine-2-carboxamide hydrochloride (160 mg) was added and stirred at room temperature for 16 h. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (DCM/MeOH=30:1) to afford the desired product (10 mg, 2.97% yield) as an off-white solid. 1H NMR (400 MHz, DMSO-d6) δ: 7.60-7.38 (m, 3H), 6.70-6.99 (m, 1H), 6.86-6.78 (m, 1H), 6.54-6.49 (m, 1H), 6.16-6.10 (m, 1H), 5.76-5.69 (m, 1H), 5.32-5.31 (m, 1H), 4.93-4.84 (m, 1H), 4.93-4.84 (m, 1H), 4.70-4.62 (m, 1H), 4.35-4.32 (m, 1H), 4.04-3.96 (m, 2H), 3.89-3.63 (m, 1H), 2.90-2.86 (m, 1H). ESI-MS m/z: 525.2[M+H]+.

後処理

  1. stirringstirred at room temperature for 16 h
  2. customThe mixture was partitioned between ethyl acetate and water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography on silica gel (DCM/MeOH=30:1)

出典と根拠

ORDレコード
ord-0eb43539e645439cab49ec1ebd22ed0b
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09227978B2

反応ノート

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