1,2-Dichloroethane → Formate

HRID 418328

반응식

HRID 418328 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([OH:7])=[O:6].[NH2:13][CH2:14][C:15]1[CH:16]=[C:17]([CH:31]=[CH:32][CH:33]=1)[C:18]([NH:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][N:28]([CH3:30])[CH3:29])=[CH:23][CH:22]=1)=[O:19].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[C:5]([NH:13][CH2:14][C:15]1[CH:33]=[CH:32][CH:31]=[C:17]([C:18](=[O:19])[NH:20][C:21]2[CH:22]=[CH:23][C:24]([CH2:27][N:28]([CH3:29])[CH3:30])=[CH:25][CH:26]=2)[CH:16]=1)=[O:7].[CH:5]([O-:7])=[O:6]

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 1699823-Chloro-p-anisic acidHCID 44819544HCID 44819544, 화합물

생성물 2

HCID 283Formate수율 423.1%HCID 25054307HCID 25054307, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A reaction vial was charged with 3-chloro-4-methoxybenzoic acid (40 mg, 0.21 mmol), 3-aminomethyl-N-(4-dimethylaminomethyl-phenyl)-benzamide (40 mg, 0.14 mmol), EDC (40 mg, 0.25 mmol) and HOBt (40 mg, 0.29 mmol). DMF (2 mL) was added followed by Hunig's base (0.11 mL, 0.57 mmol). The mixture was stirred at room temperature for 16 h. The product was purified by preparative HPLC using an acetonitrile/water/formic acid gradient providing the title compound as a formate salt (20 mg, 31% yield); MS, electrospray, 452 (M+H).

후처리

  1. customA reaction
  2. customThe product was purified by preparative HPLC

출처 및 근거

ORD 기록
ord-332f0387552244a0a63ba1c192ea222c
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093266B2

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