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Diisopropylethylamine → (R)-ethyl 4-(3'-chlorobiphenyl-4-yl)-3-(2-(ethoxycarbonylamino)acetamido)butanoate

HRID 881821
ノート
印刷プレビュー

反応式

HRID 881821 の反応式
Cl.[NH2:2][C@H:3]([CH2:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[CH:18]=2)=[CH:13][CH:12]=1)[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH2:24]([O:26][C:27]([NH:29][CH2:30][C:31](O)=[O:32])=[O:28])[CH3:25].CCN=C=NCCCN(C)C.Cl.CCN(C(C)C)C(C)C.C1C=NC2N(O)N=NC=2C=1>CN(C=O)C.O>[Cl:23][C:19]1[CH:18]=[C:17]([C:14]2[CH:15]=[CH:16][C:11]([CH2:10][C@@H:3]([NH:2][C:31](=[O:32])[CH2:30][NH:29][C:27]([O:26][CH2:24][CH3:25])=[O:28])[CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:12][CH:13]=2)[CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 81531DiisopropylethylamineHCID 96472Glycine, N-(ethoxycarbonyl)-HCID 181649HOAtHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 86648190(R)-ethyl 3-amino-4-(3'-chlorobiphenyl-4-yl)butanoate hydrochloride

生成物 1

HCID 59607590
(R)-ethyl 4-(3'-chlorobiphenyl-4-yl)-3-(2-(ethoxycarbonylamino)acetamido)butanoate
収率 73.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of (R)-ethyl 3-amino-4-(3′-chlorobiphenyl-4-yl)butanoate hydrochloride (173 mg, 0.488 mmol), 2-(ethoxycarbonylamino)acetic acid (86 mg, 0.488 mmol), EDCl (140 mg, 0.732 mmol), DIPEA (0.128 ml, 0.732 mmol) and HOAt (100 mg, 0.732 mmol) in DMF (2.5 ml) is allowed to stir at room temperature for 1 hour. The reaction mixture is diluted with water, and then the precipitated solid is collected on a funnel, washed with H2O, and dried under reduced pressure to give crude. The obtained residue is purified by silica gel flash column chromatography (heptane/EtOAc=100:0 to 0:100) to give (R)-ethyl 4-(3′-chlorobiphenyl-4-yl)-3-(2-(ethoxycarbonylamino)acetamido)butanoate (161 mg); HPLC retention time=1.16 minutes (condition B); MS (m+1)=447.3; 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.25 (t, J=7.07 Hz, 3 H) 1.29 (t, J=7.07 Hz, 3 H) 2.50 (A of ABX, Jab=16.2 Hz, Jax=5.3 Hz, 1 H) 2.54 (B of ABX, Jab=16.2 Hz, Jbx=5.3 Hz, 1 H) 2.89 (A of ABX, Jab=13.6 Hz, Jax=7.8 Hz, 1 H) 2.99 (B of ABX, Jab=13.6 Hz, Jbx=6.6 Hz, 1 H) 3.80 (be d, J=5.8 Hz, 2 H) 4.12-4.23 (m, 4 H) 4.48-4.56 (m, 1 H) 5.15 (br s, 1 H) 6.64 (br d, J=8.8 Hz, 1 H) 7.25-7.27 (m, 2 H) 7.29-7.38 (m, 2 H) 7.43-7.46 (m, 1 H) 7.49-7.52 (m, 2 H) 7.55-7.56 (m, 1 H).

後処理

  1. customthe precipitated solid is collected on a funnel
  2. washwashed with H2O
  3. customdried under reduced pressure
  4. customto give crude
  5. customThe obtained residue is purified by silica gel flash column chromatography (heptane/EtOAc=100:0 to 0:100)

出典と根拠

ORDレコード
ord-2fc36b118fac443eb3e94fe806d7613e
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08993631B2

反応ノート

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