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Trityl chloride → HCID 44195635, 화합물

HRID 2368519
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HRID 2368519 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

HCID 44195635HCID 44195635, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(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.

후처리

  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)

출처 및 근거

ORD 기록
ord-de829064745f4cba881fb4375232ffb5
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703776B2

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