1,2-Dichloroethane → HCID 178481254, 화합물

HRID 230007노트

반응식

HRID 230007 반응식
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([N:11]([CH2:23][C:24]2[CH:32]=[CH:31][C:27]([C:28]([OH:30])=O)=[CH:26][CH:25]=2)[C:12]2[N:16]([CH3:17])[C:15]3[CH:18]=[CH:19][C:20]([OH:22])=[CH:21][C:14]=3[N:13]=2)[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].O.[NH:34]1[C:38]([NH2:39])=[N:37][N:36]=[N:35]1.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C.C(Cl)CCl>CN(C=O)C>[C:1]([CH:5]1[CH2:6][CH2:7][CH:8]([N:11]([CH2:23][C:24]2[CH:25]=[CH:26][C:27]([C:28]([NH:39][C:38]3[NH:37][N:36]=[N:35][N:34]=3)=[O:30])=[CH:31][CH:32]=2)[C:12]2[N:16]([CH3:17])[C:15]3[CH:18]=[CH:19][C:20]([OH:22])=[CH:21][C:14]=3[N:13]=2)[CH2:9][CH2:10]1)([CH3:2])([CH3:3])[CH3:4]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 688361734-{[(4-Tert-butylcyclohexyl)(5-hydroxy-1-methyl-1h-benzimidazol-2-yl)amino]methyl}benzoic acidHCID 178509300HCID 178509300, 화합물

생성물 1

HCID 178481254HCID 178481254, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
40 °C

실험 절차

To a solution of the title compound of Example 15 Step B (0.02 mmol, 10 mg), 1H-tetraazol-5-amine monohydrate (0.2 mmol, 21 mg), HOBt (0.2 mmol, 31 mg) and DIEA (0.3 mmol, 52 μL) in 0.5 mL of DMF was added EDC (0.2 mmol, 38 mg). The reaction was heated to 40° C. 15 min, then allowed to stand at ambient temperature overnight. The reaction mixture was 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 503 (M+H). HPLC A: 1.88 min.

후처리

  1. custom15 min
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. custompurified by reverse-phase chromatography (Condition B)

출처 및 근거

ORD 기록
ord-27b2d7bd8e024422a541cee6563365ea
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563815B2

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