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Triethylamine → HCID 53930965, 화합물

HRID 582165
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HRID 582165 반응식
[Br:1]Br.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O[CH2:23][C:24]#[C:25][C:26]1[N:30]=[CH:29][N:28]([C:31]([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[N:27]=1.C(N(CC)CC)C>ClCCl>[Br:1][CH2:23][C:24]#[C:25][C:26]1[N:30]=[CH:29][N:28]([C:31]([C:44]2[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=2)([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[N:27]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 24408BromineHCID 54249207HCID 54249207, 화합물

생성물 1

HCID 53930965HCID 53930965, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

반응 조건

온도
0 °C

실험 절차

A solution of bromine (1.72 ml) in dry dichloromethane (10 ml) was added dropwise to a stirred, cooled (-5° C.), solution of triphenylphosphine (8.74 g) in dry dichloromethane (140 ml) whilst maintaining the temperature below 0° C. The solution was stirred for a further ten minutes at 0° C., then treated dropwise over one hour with a solution of the above alcohol (12.17 g) and triethylamine (4.64 ml) in dry dichloromethane (200 ml). After ten minutes, the mixture was evaporated under reduced pressure and the residue chromatographed on silica, using dichloromethane-ether (25:2) as eluant, to give 1-bromo-3(1-trityl-1,2,4-triazol-3-yl)prop-2-yne (8.10 g, m.p. 181-183° C. dec). NMR (CDCl3): δ 4.1(2H,s), 7.05-7.35(15H,m), 7.95(1H,s). M/S: M+ 427,429.

후처리

  1. temperaturewhilst maintaining the temperature below 0° C
  2. waitAfter ten minutes
  3. customthe mixture was evaporated under reduced pressure
  4. customthe residue chromatographed on silica

출처 및 근거

ORD 기록
ord-ecf9fed3ab944052af1c2c770779f642
출처 데이터셋
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05922644

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