Ethanol → HCID 178486160, 화합물

HRID 1190141노트

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HRID 1190141 반응식
[CH3:1][C:2]1([CH3:40])[CH2:7][CH2:6][C:5]([C:8]2[CH:13]=[C:12]([CH2:14][CH2:15][S:16](=[O:21])(=[O:20])[N:17]([CH3:19])[CH3:18])[CH:11]=[CH:10][C:9]=2[NH:22][C:23]([C:25]2[N:26](COCC[Si](C)(C)C)[CH:27]=[C:28]([C:30]#[N:31])[N:29]=2)=[O:24])=[CH:4][CH2:3]1.CCO.C(O)(C(F)(F)F)=O.CO>C(Cl)Cl>[CH3:1][C:2]1([CH3:40])[CH2:7][CH2:6][C:5]([C:8]2[CH:13]=[C:12]([CH2:14][CH2:15][S:16](=[O:21])(=[O:20])[N:17]([CH3:19])[CH3:18])[CH:11]=[CH:10][C:9]=2[NH:22][C:23]([C:25]2[NH:26][CH:27]=[C:28]([C:30]#[N:31])[N:29]=2)=[O:24])=[CH:4][CH2:3]1

참가 물질

6

반응물 4

HCID 702EthanolHCID 887MethanolHCID 6422Trifluoroacetic acidHCID 589944264-Cyano-1-(2-trimethylsilanyl-ethoxymethyl)-1H-imidazole-2-carboxylic acid [2-(4,4-dimethyl-cyclohex-1-enyl)-4-(2-dimethylsulfamoyl-ethyl)-phenyl]-amide

생성물 1

HCID 178486160HCID 178486160, 화합물수율 61.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 355 mg (0.606 mmol) of 4-cyano-1-(2-trimethylsilanyl-ethoxymethyl)-1H-imidazole-2-carboxylic acid [2-(4,4-dimethyl-cyclohex-1-enyl)-4-(2-dimethylsulfamoyl-ethyl)-phenyl]-amide (as prepared in the previous step) in CH2Cl2 (15 mL) was treated with EtOH (300 μL) and TFA (1.5 mL) at RT for 24 h. MeOH (20 mL) was added, and the solvents were evaporated in vacuo. The solid was triturated with acetonitrile to afford 169 mg (61%) of the title compound as a white solid: 1H-NMR (CD3CN; 400 MHz): δ 9.41 (s, 1H), 8.23 (d, 1H, J=8.0 Hz), 7.91 (s, 1H), 7.22 (d, 1H, J=8.0 Hz), 7.18 (s, 1H), 5.80-5.71 (m, 1H), 3.31-3.21 (m, 2H), 3.10-3.00 (m, 2H), 2.85 (s, 6H), 2.37-2.27 (m, 2H), 2.10-2.04 (m, 2H), 1.64-1.55 (m, 2H), 1.10 (s, 6H). Mass spectrum (ESI, m/z): Calcd. for C23H29N5O3S, 456.2 (M+H). found 456.1.

후처리

  1. customthe solvents were evaporated in vacuo
  2. customThe solid was triturated with acetonitrile

출처 및 근거

ORD 기록
ord-f7fc930e5d0947a0b28594ac41bc86ba
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674100B2

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