Triethylamine → HCID 178443160、化合物

HRID 903304ノート

反応式

HRID 903304 の反応式
[CH2:1]([O:15][C:16]1[CH:25]=[CH:24][CH:23]=[CH:22][C:17]=1[C:18](=[O:21])[CH2:19]Br)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[NH:26]1[CH:30]=[N:29][N:28]=[N:27]1.C(N(CC)CC)C>C(#N)C>[NH:26]1[C:30]([CH2:19][C:18]([C:17]2[CH:22]=[CH:23][CH:24]=[CH:25][C:16]=2[O:15][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])=[O:21])=[N:29][N:28]=[N:27]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 20516628HCID 20516628、化合物HCID 178418441HCID 178418441、化合物

生成物 1

HCID 178443160HCID 178443160、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

To a solution of 14.6 g of o-tetradecyloxyphenacylbromide in 75 ml of acetonitrile was added a solution of 2.8 g of tetrazole and 4.0 g of triethylamine in 75 ml of acetonitrile. The reaction mixture was stirred at reflux temperature for 2 hours then evaporated to dryness. The residue was dissolved in chloroform and the organic layer washed with water, dried over magnesiumsulfate, filtered and evaporated to give the crude compound. Recrystallisation from petrol (b.p. 60°-80° C.) gave the acetophenone derivative as a fine white powder. Yield: 12.7 g; m.p. 67° to 69° C.

後処理

  1. temperatureat reflux temperature for 2 hours
  2. customthen evaporated to dryness
  3. dissolutionThe residue was dissolved in chloroform
  4. washthe organic layer washed with water
  5. dry with materialdried over magnesiumsulfate
  6. filtrationfiltered
  7. customevaporated
  8. customto give the crude compound
  9. customRecrystallisation from petrol (b.p. 60°-80° C.)

出典と根拠

ORDレコード
ord-1c134ee3be2a42ecaedc855b2a855812
出典データセット
uspto-grants-1980_10
特許番号
US04226934

反応ノート

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