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Trityl chloride → 3-Methyl-1-trityl-1H-1,2,4-triazole

HRID 275542
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HRID 275542 반응식
[C:1](Cl)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:21][C:22]1[N:26]=[CH:25][NH:24][N:23]=1.C(N(CC)CC)C>ClCCl>[C:1]([N:24]1[CH:25]=[N:26][C:22]([CH3:21])=[N:23]1)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 178433329HCID 178433329, 화합물

생성물 1

HCID 543633743-Methyl-1-trityl-1H-1,2,4-triazole수율 86.6%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Trityl chloride (19.0 g) was added portionwise to a stirred solution of 3-methyl-1,2,4-triazole (5.6 g, commercial) and triethylamine (9.5 ml) in dichloromethane (200 ml). The mixture was diluted with dichloromethane (100 ml), washed with water (50 ml), dried over magnesium sulphate and evaporated under reduced pressure to give 1-trityl-3-methyl-1,2,4-triazole (19.0 g). Recrystallisation of a 2 g sample from toluene-hexane (1:1) gave pure material (1.32 g, m.p. 194°-196° C.). NMR (CDCl3): δ2.41(3H,s), 7.03-7.40(15H,m), 7.83(1H,s).

후처리

  1. washwashed with water (50 ml)
  2. dry with materialdried over magnesium sulphate
  3. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-179d6db53ff04657a29af395362a53ce
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05393732

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