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1,2-Dichloroethane → N-(3,3-Dimethylbutyl)-2-[3-(2,2-dimethylpropanoyl)-6-methoxy-1H-indazol-1-yl]-N-ethylacetamide

HRID 490806
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HRID 490806 반응식
[CH3:1][C:2]([CH3:21])([CH3:20])[C:3]([C:5]1[C:13]2[C:8](=[CH:9][C:10]([O:14][CH3:15])=[CH:11][CH:12]=2)[N:7]([CH2:16][C:17]([OH:19])=O)[N:6]=1)=[O:4].C1C=C[C:25]2N(O)N=N[C:26]=2[CH:27]=1.[CH2:32](Cl)CCl.CC[N:38]([CH:42]([CH3:44])C)[CH:39]([CH3:41])C>CN(C=O)C>[CH3:32][C:26]([CH3:25])([CH3:27])[CH2:44][CH2:42][N:38]([CH2:39][CH3:41])[C:17](=[O:19])[CH2:16][N:7]1[C:8]2[C:13](=[CH:12][CH:11]=[C:10]([O:14][CH3:15])[CH:9]=2)[C:5]([C:3](=[O:4])[C:2]([CH3:21])([CH3:20])[CH3:1])=[N:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 57675531[3-(2,2-Dimethylpropanoyl)-6-methoxy-1H-indazol-1-yl]acetic acid

생성물 1

HCID 10341009N-(3,3-Dimethylbutyl)-2-[3-(2,2-dimethylpropanoyl)-6-methoxy-1H-indazol-1-yl]-N-ethylacetamide

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

To a solution of 29.0 mg [3-(2,2-dimethylpropanoyl)-6-methoxy-1H-indazol-1-yl]acetic acid in 1 mL DMF was added 23.0 mg HOBt, 32.3 mg N-Ethyl-3,3-dimethylbutan-1-lamine hydrochloride from the Step A above, 38.3 mg EDC, and 45.2 mg DIEA in that order. The mixture was stirred at room temperature for four hours and heated at 45° C. over night and purified by RP-HPLC using 70-100% MeCN gradient. The pure product fractions were pooled and lyophilized to give the title compound. LC-MS: 4.29 min. (m/Z=402.4, 424.3).

후처리

  1. temperatureheated at 45° C. over night
  2. custompurified by RP-HPLC using 70-100% MeCN gradient

출처 및 근거

ORD 기록
ord-5e23dd7656594e2dbf304fa91e168f28
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528163B2

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