Triethylamine → 1-(4-Chlorobutoxymethyl)-2-bromo-4,5-dichloroimidazole

HRID 979511노트

반응식

HRID 979511 반응식
[Br:1][C:2]1[NH:3][C:4]([Cl:8])=[C:5]([Cl:7])[N:6]=1.C(N(CC)CC)C.[Cl:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][CH2:22]Cl>C1(C)C=CC=CC=1>[Cl:16][CH2:17][CH2:18][CH2:19][CH2:20][O:21][CH2:22][N:3]1[C:4]([Cl:8])=[C:5]([Cl:7])[N:6]=[C:2]1[Br:1]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 994842-Bromo-4,5-dichloro-1H-imidazoleHCID 3146301-Chloro-4-(chloromethoxy)butane

생성물 1

HCID 137726871-(4-Chlorobutoxymethyl)-2-bromo-4,5-dichloroimidazole수율 35.6%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a mixture of 1.08 g of 2-bromo-4,5-dichloroimidazole, 0.51 g of triethylamine and about 30 ml of toluene was added dropwise 0.79 g of 4-chlorobutoxymethyl chloride at room temperature, and the resulting mixture was stirred at room temperature for 2 hours. The deposited crystal was filtered off and washed with about 10 ml of toluene. The filtrate thus obtained was concentrated under reduced pressure, and the residual oily product was purified by column chromatography on silica gel to obtain 0.60 g of 1-(4-chlorobutoxymethyl)-2-bromo-4,5-dichloroimidazole.

후처리

  1. filtrationThe deposited crystal was filtered off
  2. washwashed with about 10 ml of toluene
  3. customThe filtrate thus obtained
  4. concentrationwas concentrated under reduced pressure
  5. customthe residual oily product was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-4b56f2c78ab2487fb6f83b09156286ee
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04668693

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