Hydrochloric Acid → HCID 13474665、化合物

HRID 1980527ノート

反応式

HRID 1980527 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 8028TetrahydrofuranHCID 13474661HCID 13474661、化合物

生成物 1

HCID 13474665HCID 13474665、化合物収率 87.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-b81dd2dd999846b7a7b3b9d78d3973d6
出典データセット
uspto-grants-1985_04
特許番号
US04510136

反応ノート

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