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Ammonium Chloride → HCID 86709394, 화합물

HRID 2172252
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HRID 2172252 반응식
CC(C)([O-])C.[Na+].Cl[C:8]1[N:9]([CH2:16][CH2:17][CH:18]([OH:44])[CH2:19][O:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]3[N:28]=[C:29]([CH2:32][C:33]4[CH:38]=[CH:37][C:36]([O:39][C:40]([F:43])([F:42])[F:41])=[CH:35][CH:34]=4)[S:30][CH:31]=3)=[CH:23][CH:22]=2)[CH:10]=[C:11]([N+:13]([O-:15])=[O:14])[N:12]=1.[Cl-].[NH4+]>CC(C)=O>[N+:13]([C:11]1[N:12]=[C:8]2[N:9]([CH:10]=1)[CH2:16][CH2:17][CH:18]([CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]3[N:28]=[C:29]([CH2:32][C:33]4[CH:38]=[CH:37][C:36]([O:39][C:40]([F:43])([F:42])[F:41])=[CH:35][CH:34]=4)[S:30][CH:31]=3)=[CH:23][CH:22]=1)[O:44]2)([O-:15])=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 23676156Sodium t-butoxide2회HCID 70874643HCID 70874643, 화합물

생성물 1

HCID 86709394HCID 86709394, 화합물수율 22.1%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Sodium tert-butoxide (62 mg) was added to a dimethyl formaldehyde solution (5 ml) of 4-(2-chloro-4-nitroimidazol-1-yl)-1-{4-[2-(4-trifluoromethoxybenzyl)thiazol-4-yl]phenoxy}butan-2-ol (334 mg), and the mixture was stirred at room temperature. While confirming the progress of the reaction, sodium tert-butoxide (62 mg) was added 3 times, and the resulting mixture was stirred overnight. A saturated ammonium chloride aqueous solution was added to the reaction mixture, and the precipitated solid was sequentially washed with water and diisopropyl ether. The residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1→ethyl acetate) to afford the title compound as a pale brown powder (69 mg).

후처리

  1. additionwas added 3 times
  2. stirringthe resulting mixture was stirred overnight
  3. washthe precipitated solid was sequentially washed with water and diisopropyl ether
  4. customThe residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:1→ethyl acetate)

출처 및 근거

ORD 기록
ord-76c0cfe0e6a94ce7a4d87f58ee2bb1e9
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051333B2

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