Hydrochloric Acid → HCID 13474665, 화합물

HRID 1980527노트

반응식

HRID 1980527 반응식
[C:1]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]=[CH:5][C:4]([Si:7]([CH3:18])([O:14]C(C)C)[CH2:8][N:9]2[CH:13]=[N:12][CH:11]=[N:10]2)=[CH:3][CH:2]=1.Cl.O.O1CCCC1>CCOCC>[C:1]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:2]=[CH:3][C:4]([Si:7]([OH:14])([CH3:18])[CH2:8][N:9]2[CH:13]=[N:12][CH:11]=[N:10]2)=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 13474661HCID 13474661, 화합물

생성물 1

HCID 13474665HCID 13474665, 화합물수율 87.5%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 3.0 g (8.9 mmol) of (1,1'-biphenyl-4-yl)methyl(2-propoxy)(1H-1,2,4-triazol-1-ylmethyl)silane, 3 ml of concentrated hydrochloric acid, 10 ml of water, and 10 ml of tetrahydrofuran was stirred at room temperature overnight. The resulting solution was diluted with ether, washed with saturated aqueous sodium bicarbonate, water, and brine, dried over magnesium sulfate, and evaporated to leave 2.3 g of viscous oil. Chromatography over silica gel, eluting with hexane followed by ether, provided 1.1 g (42%) of the title compound as a viscous oil that solidified on standing: m.p. 97°-99°; nmr (CDCl3) 0.5 (3H, s), 3.9 (2H, s), 5.2 (1H, broad s), 7.3-7.8 (9H, m), 7.9 (1H, s), 8.0 (1H, s).

후처리

  1. washwashed with saturated aqueous sodium bicarbonate, water, and brine
  2. dry with materialdried over magnesium sulfate
  3. customevaporated

출처 및 근거

ORD 기록
ord-b81dd2dd999846b7a7b3b9d78d3973d6
출처 데이터셋
uspto-grants-1985_04
특허 번호
US04510136

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