Imidazole → HCID 23499597, 화합물

HRID 1836549노트

반응식

HRID 1836549 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][OH:16])=[CH:11][C:10]=1[Br:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C=CN=C1.[C:23]([Si:27](Cl)([CH3:29])[CH3:28])([CH3:26])([CH3:25])[CH3:24].O>CN(C=O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH2:15][O:16][Si:27]([C:23]([CH3:26])([CH3:25])[CH3:24])([CH3:29])[CH3:28])=[CH:11][C:10]=1[Br:17])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 962WaterHCID 28928tert-Butyldimethylsilyl chlorideHCID 17439222HCID 17439222, 화합물

생성물 1

HCID 23499597HCID 23499597, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3.0 g (10.23 mmol) of [4-(benzyloxy)-3-bromophenyl]methanol (Example I) are initially charged in 30 ml of DMF. At room temperature, 1.39 g (12.28 mmol) of 1H-imidazole (60% pure) and 2.01 g (13.3 mmol) of tert-butyl(chloro)dimethylsilane are added. The reaction mixture is stirred at room temperature overnight. Water is then added, and the mixture is extracted three times with diethyl ether. The combined organic phases are washed three times with water and once with saturated sodium chloride solution. The organic phase is dried with sodium sulphate and the solvent is removed under reduced pressure. This gives 4.02 g (86% of theory) of {[4-(benzyloxy)-3-bromobenzyl]oxy}(tert-butyl)dimethylsilane.

후처리

  1. extractionthe mixture is extracted three times with diethyl ether
  2. washThe combined organic phases are washed three times with water
  3. dry with materialThe organic phase is dried with sodium sulphate
  4. customthe solvent is removed under reduced pressure

출처 및 근거

ORD 기록
ord-dbf5bce86c70495380ad6baab3b04383
출처 데이터셋
uspto-grants-2004_08
특허 번호
US06777442B2

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