1,2-Dichloroethane → HCID 72375749、化合物

HRID 2173438ノート

反応式

HRID 2173438 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:13][C:14]([OH:16])=O)[CH:5]=[CH:6][C:7]=1[N:8]1[CH:12]=[N:11][N:10]=[N:9]1.[N:17]1([CH2:23][CH2:24][C:25]2[CH:34]=[CH:33][C:28]3[C:29](=[O:32])[O:30][CH2:31][C:27]=3[CH:26]=2)[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>C(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([CH2:13][C:14]([N:20]2[CH2:21][CH2:22][N:17]([CH2:23][CH2:24][C:25]3[CH:34]=[CH:33][C:28]4[C:29](=[O:32])[O:30][CH2:31][C:27]=4[CH:26]=3)[CH2:18][CH2:19]2)=[O:16])[CH:5]=[CH:6][C:7]=1[N:8]1[CH:12]=[N:11][N:10]=[N:9]1

参加物

6

反応物 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 595686715-[2-(piperazin-1-yl)ethyl]-2-benzofuran-1(3H)-oneHCID 67517239HCID 67517239、化合物

生成物 1

HCID 72375749HCID 72375749、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of [3-fluoro-4-(1H-tetrazol-1-yl)phenyl]acetic acid (0.68 mmol) in 10 mL of anhydrous DCM was added 5-(2-piperazin-1-ylethyl)-2-benzofuran-1(3H)-one (191 mg, 0.68 mmol), EDC (200 mg, 1.01 mmol), HOBt (136 mg, 1.01 mmol), TEA (341 mg, 3.38 mmol) was stirred at ambient temperature overnight. The mixture was added DCM, washed with brine, the organic layer was dried over anhydrous Na2SO4 and concentrated. The residue was purified via prep-TLC to give the title compound. 1H-NMR (400 MHz, CDCl3) δ ppm 8.84 (s, 1H), 7.82 (d, J=7.8 Hz, 1H), 7.31˜737 (m, 3H), 7.11˜7.19 (m, 2H), 5.29 (s, 2H), 3.59 (s, 2H), 3.49˜3.52 (m, 2H), 3.37˜3.4 (m, 2H), 2.89˜2.93 (m, 2H), 2.64˜2.68 (m, 2H), 2.4˜2.45 (m, 4H).

後処理

  1. washwashed with brine
  2. dry with materialthe organic layer was dried over anhydrous Na2SO4
  3. concentrationconcentrated
  4. customThe residue was purified via prep-TLC

出典と根拠

ORDレコード
ord-0c8a36f661ce4f6ab5a7e497ca1420ba
出典データセット
uspto-grants-2015_06
特許番号
US09056859B2

反応ノート

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