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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Water → HCID 66939361、化合物

HRID 1257422
ノート
印刷プレビュー

反応式

HRID 1257422 の反応式
[OH:1][N:2]=[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([C:11]([F:14])([F:13])[F:12])[CH:6]=1)[NH2:4].Cl[C:16](=O)[CH2:17][N:18]1[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]1.O>N1C=CC=CC=1>[F:14][C:11]([F:13])([F:12])[C:7]1[CH:6]=[C:5]([C:3]2[N:4]=[C:16]([CH2:17][N:18]3[CH:22]=[C:21]([C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH:20]=[N:19]3)[O:1][N:2]=2)[CH:10]=[CH:9][CH:8]=1
参加物反応条件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 962WaterHCID 609330N'-hydroxy-3-(trifluoromethyl)benzimidamideHCID 58127969HCID 58127969、化合物

生成物 1

HCID 66939361HCID 66939361、化合物収率 10.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
115 °C

実験手順

A solution of N′-hydroxy-3-(trifluoromethyl)benzenecarboximidamide (2.1 g) in pyridine (20 mL) was cooled in an ice bath, and the compound (2.3 g) obtained in Example 115c was added. The reaction mixture was stirred overnight with heating at 110-120° C. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was separated, washed successively with 1N hydrochloric acid and saturated brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate) to give the title compound (0.38 g) as a solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe ethyl acetate layer was separated
  3. washwashed successively with 1N hydrochloric acid and saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography (carrier: silica gel, eluent: petroleum ether-ethyl acetate)

出典と根拠

ORDレコード
ord-bbb7264266f546f2b8552eebeb0808ec
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461348B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート