Water → 2-(2-{2-[4-(4-Chloro-1,2-diphenyl-but-1-enyl)-phenoxy]ethoxy}-ethoxy)-tetrahydropyran

HRID 2068229노트

반응식

HRID 2068229 반응식
[Cl:1][CH2:2][CH2:3][C:4]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[C:5]([C:12]1[CH:17]=[CH:16][C:15]([OH:18])=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[H-].[Na+].I[CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH:34]1[CH2:39][CH2:38][CH2:37][CH2:36][O:35]1.O>O1CCCC1>[Cl:1][CH2:2][CH2:3][C:4]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=[C:5]([C:12]1[CH:13]=[CH:14][C:15]([O:18][CH2:28][CH2:29][O:30][CH2:31][CH2:32][O:33][CH:34]2[CH2:39][CH2:38][CH2:37][CH2:36][O:35]2)=[CH:16][CH:17]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 5588852H-Pyran, tetrahydro-2-[2-(2-iodoethoxy)ethoxy]-HCID 539047244-[(1Z)-4-Chloro-1,2-diphenylbut-1-en-1-yl]phenol

생성물 1

HCID 668526812-(2-{2-[4-(4-Chloro-1,2-diphenyl-but-1-enyl)-phenoxy]ethoxy}-ethoxy)-tetrahydropyran

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4-(4-Chloro-1,2-diphenyl-but-1-enyl)phenol (0.33 g, 0.001 mol) was dissolved in tetrahydrofuran (3 ml) under a nitrogen atmosphere. Sodium hydride (0.036 g, 0.0015 mol) was added to the solution and the mixture was stirred at room temperature for an hour. 2-[2-(2-iodo-ethoxy)-ethoxy)-tetrahydropyran (0.6 g, 0.002 mol) was added and the mixture was refluxed for 3 hours. After cooling and adding water the mixture was extracted three times with ethyl acetate. The organic phase was dried with sodium sulphate and evaporated to dryness. The residue was used in the next reaction step without further purification.

후처리

  1. temperaturethe mixture was refluxed for 3 hours
  2. temperatureAfter cooling
  3. extractionwas extracted three times with ethyl acetate
  4. dry with materialThe organic phase was dried with sodium sulphate
  5. customevaporated to dryness
  6. customThe residue was used in the next reaction step without further purification

출처 및 근거

ORD 기록
ord-a68c4b42839949f9af12aceadeb34c50
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293947B2

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