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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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Trityl chloride → HCID 44195635、化合物

HRID 2368519
ノート
印刷プレビュー

反応式

HRID 2368519 の反応式
[C:1](/[N:4]=[CH:5]/[N:6]([CH3:8])[CH3:7])(=[S:3])[NH2:2].[C:9](Cl)([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>ClCCl>[CH3:7][N:6]([CH3:8])/[CH:5]=[N:4]/[C:1](=[S:3])[NH:2][C:9]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1)[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6456Trityl chlorideHCID 9631647[N(E)]-N-[(Dimethylamino)methylene]thiourea

生成物 1

HCID 44195635HCID 44195635、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(E)-N′-carbamothioyl-N,N-dimethylformimidamide (63) (5 g, 38 mmol), tritylchloride (11.6 g, 41.8 mmol) and trietheylamine (16 mL, 114 mmol) were refluxed in dichloromethane overnight. The reaction mixture was cooled to room temperature and filtered through a plug of celite. The resulting filtrate was washed with saturated sodium bicarbonate solution, followed with brine. The organic layer was dried with sodium sulfate, filtered and concentrated in vacuo. The residue was purified by flash chromatography on silica gel column (40%-100% EtOAc in hexanes) to afford (E)-N,N-dimethyl-N′-(tritylcarbamothioyl) formimidamide (64) as a white solid.

後処理

  1. filtrationfiltered through a plug of celite
  2. washThe resulting filtrate was washed with saturated sodium bicarbonate solution
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash chromatography on silica gel column (40%-100% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-de829064745f4cba881fb4375232ffb5
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08703776B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート