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Ammonium Chloride → HCID 86709394、化合物

HRID 2172252
ノート
印刷プレビュー

反応式

HRID 2172252 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 23676156Sodium t-butoxide2 回HCID 70874643HCID 70874643、化合物

生成物 1

HCID 86709394HCID 86709394、化合物収率 22.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-76c0cfe0e6a94ce7a4d87f58ee2bb1e9
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09051333B2

反応ノート

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