1,2-Dichloroethane → HCID 178441009, 화합물

HRID 229984노트

반응식

HRID 229984 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([OH:28])=O)=[CH:24][CH:23]=1)[CH:11]1[CH2:16][CH2:15][CH:14]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH2:13][CH2:12]1.O.[NH:32]1[C:36]([NH2:37])=[N:35][N:34]=[N:33]1.C1C=CC2N(O)N=NC=2C=1.C(Cl)CCl.CCN(C(C)C)C(C)C>CN(C=O)C>[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[C:2]1[N:10]([CH2:21][C:22]1[CH:30]=[CH:29][C:25]([C:26]([NH:37][C:36]2[NH:35][N:34]=[N:33][N:32]=2)=[O:28])=[CH:24][CH:23]=1)[CH:11]1[CH2:12][CH2:13][CH:14]([C:17]([CH3:18])([CH3:20])[CH3:19])[CH2:15][CH2:16]1

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 688356554-{[1h-Benzimidazol-2-yl(4-tert-butylcyclohexyl)amino]methyl}benzoic acidHCID 178509300HCID 178509300, 화합물

생성물 1

HCID 178441009HCID 178441009, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of the title compound of Example 1 Step D (0.1 mmol, 41 mg), 1H-tetraazol-5-amine monohydrate (0.2 mmol, 21 mg), HOBt (0.25 mmol, 38 mg) and EDC (0.4 mmol, 77 mg) in 1 mL of DMF was added DIEA (0.5 mmol, 90 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, acidified with TFA, and purified by reverse-phase chromatography (Condition A). Lyophilization afforded the product as a white solid. MS (ESI): m/z 473 (M+H). HPLC A: 1.86 min.

후처리

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

출처 및 근거

ORD 기록
ord-b01727d900174c28bb3b64a0cb95989e
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563815B2

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