Triethylamine → HCID 178443160, 화합물

HRID 903304노트

반응식

HRID 903304 반응식
[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

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 20516628HCID 20516628, 화합물HCID 178418441HCID 178418441, 화합물

생성물 1

HCID 178443160HCID 178443160, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-1c134ee3be2a42ecaedc855b2a855812
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04226934

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