Diethyl Ether → HCID 68660307、化合物

HRID 1773052

反応式

HRID 1773052 の反応式
[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH2:13][OH:14])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][CH2:16][O:17][CH2:18][CH3:19]>CC[N+](CC1C=CC=CC=1)(CC)CC.[Cl-].C1(C)C=CC=CC=1.[OH-].[Na+]>[CH2:1]([N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH2:13][O:14][CH2:19][CH2:18][O:17][CH:16]=[CH2:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 2

HCID 3283Diethyl EtherHCID 311778(1-benzyl-1H-imidazol-2-yl)methanol

生成物 1

HCID 68660307HCID 68660307、化合物収率 85%

試薬・触媒・溶媒 3

HCID 66133Benzyl triethylammonium chloride触媒HCID 1140Toluene溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

0.54 g of TEBAC (2.4×10−3 mol) and 5.6 g of CEVE (0.05 mol) are added to a solution of 1-benzyl-2-hydroxymethylimidazole (4.7 g, 0.024 mol.) in toluene (15 ml). A basic solution 20 N in NaOH (100 ml) is then added in the medium and the heterogeneous mixture is brought to 90° C. for 24 h with vigorous stirring. After cooling, the solution is diluted with 250 ml of decanted ether, then the organic phase is washed with water until pH=7 (10×100 ml). The organic phase is dried on Na2SO4, filtered, then evaporated under reduced pressure to yield 5.3 g (85%) of desired product. Given the satisfactory purity of the obtained product, no further purification is required.

後処理

  1. temperatureAfter cooling
  2. washthe organic phase is washed with water until pH=7 (10×100 ml)
  3. customThe organic phase is dried on Na2SO4
  4. filtrationfiltered
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-19ffd579d44d4a55829791c022dcd017
出典データセット
uspto-grants-2016_02
特許番号
US09252446B2

関連ノート

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