1,2-Dichloroethane → HCID 178441008、化合物

HRID 229995ノート

反応式

HRID 229995 の反応式
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([N:11]([CH2:24][C:25]2[CH:33]=[CH:32][C:28]([C:29]([OH:31])=O)=[CH:27][CH:26]=2)[C:12]2[N:16]([CH2:17][CH2:18][OH:19])[C:15]3[CH:20]=[CH:21][CH:22]=[CH:23][C:14]=3[N:13]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].O.[NH:35]1[C:39]([NH2:40])=[N:38][N:37]=[N:36]1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.CCN(C(C)C)C(C)C>CN(C=O)C>[C:1]([CH:5]1[CH2:6][CH2:7][CH:8]([N:11]([CH2:24][C:25]2[CH:26]=[CH:27][C:28]([C:29]([NH:40][C:39]3[NH:38][N:37]=[N:36][N:35]=3)=[O:31])=[CH:32][CH:33]=2)[C:12]2[N:16]([CH2:17][CH2:18][OH:19])[C:15]3[CH:20]=[CH:21][CH:22]=[CH:23][C:14]=3[N:13]=2)[CH2:9][CH2:10]1)([CH3:3])([CH3:4])[CH3:2]

参加物

7

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 688378984-{[(4-Tert-butylcyclohexyl)(1-{2-hydroxyethyl}-1h-benzimidazol-2-yl)-amino]methyl}benzoic acidHCID 178509300HCID 178509300、化合物

生成物 1

HCID 178441008HCID 178441008、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of the title compound of Example 10 Step B (0.04 mmol, 19 mg) 1H-tetraazol-5-amine monohydrate (0.13 mmol, 13 mg), HOBt (0.085 mmol, 13 mg) and EDC (0.17 mmol, 33 mg) in 0.5 mL of DMF was added DIEA (0.21 mmol, 36 μL). The reaction mixture was allowed to stand at ambient temperature overnight, then concentrated under reduced pressure. The residue was taken up in ca. 2:1 dioxane/H2O and acidified with TFA, then purified by reverse-phase chromatography (Condition B). The product was lyophilized, affording the title compound as a white solid. MS (ESI): m/z 517 (M+H). HPLC A: 1.81 min.

後処理

  1. concentrationconcentrated under reduced pressure
  2. custompurified by reverse-phase chromatography (Condition B)

出典と根拠

ORDレコード
ord-131c5d630577494eb04e6d088c9a28db
出典データセット
uspto-grants-2009_07
特許番号
US07563815B2

反応ノート

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