홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ammonium Chloride → 3-[2-(4,5-Diphenyl-2-thiazolyl)ethyl]phenol

HRID 1461757
노트
인쇄 미리보기

반응식

HRID 1461757 반응식
C([Li])CCC.[CH3:6][C:7]1[S:8][C:9]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[N:11]=1.Br[CH2:25][C:26]1[CH:27]=[C:28]([CH:37]=[CH:38][CH:39]=1)[O:29][Si](C)(C)C(C)(C)C.[Cl-].[NH4+].[F-].C([N+](CCCC)(CCCC)CCCC)CCC>CCCCCC.C1COCC1.Cl.C(OCC)C>[C:12]1([C:10]2[N:11]=[C:7]([CH2:6][CH2:25][C:26]3[CH:27]=[C:28]([OH:29])[CH:37]=[CH:38][CH:39]=3)[S:8][C:9]=2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 25517Ammonium ChlorideHCID 773652-Methyl-4,5-diphenylthiazoleHCID 2724141Tetrabutylammonium FluorideHCID 10040514[3-(Bromomethyl)phenoxy](tert-butyl)dimethylsilaneHCID 178418339Butyllithium

생성물 1

HCID 150069043-[2-(4,5-Diphenyl-2-thiazolyl)ethyl]phenol수율 58%

시약·촉매·용매 4

HCID 313Hydrochloric Acid용매HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매4회HCID 8058Hexane용매

반응 조건

온도
-78 °C

실험 절차

n-Butyllithium (1.53 g, 24 mmol) in hexane (9.5 mL) was added dropwise to a stirred solution of 2-methyl-4,5-diphenylthiazole (5 g, 20 mmol) in dry THF (150mL,) maintained at -78° C. under an atmosphere of nitrogen. After 25 minutes a solution of [3-(bromomethyl)phenoxy]dimethyl(1,1-dimethylethyl)silane (6.60 g, 22mmol) in THF (10mL) was added dropwise, the mixture stirred at -78° C. for 10 minutes and the allowed to warm to room temperature. The reaction mixture was poured onto saturated ammonium chloride solution, extracted with CH2Cl2, the extracts combined, dried over sodium sulfate and concentrated in vacuo to leave an oil which was dissolved in THF (25 mL). A solution of tetra-n-butylammonium fluoride (6.77 g, 26 mmol) in THF (25.86 mL) was added and the mixture stirred at room temperature for 30 minutes before being diluted with 1N HCl solution (100 mL). The mixture was extracted with CH2Cl2, the combined extracts dried over sodium sulfate and concentrated to leave an oil. Chromatography on a column of silica gel using a mixture of hexanes and diethyl ether (2:1) as eluent furnished 3-[2-(4,5-diphenyl-2-thiazolyl)ethyl]phenol (4.13 g, 58%), mp 166°-168° C. after recrystallization from a mixture of hexanes and CH2Cl2.

후처리

  1. temperatureto warm to room temperature
  2. extractionextracted with CH2Cl2
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customto leave an oil which
  6. stirringthe mixture stirred at room temperature for 30 minutes
  7. extractionThe mixture was extracted with CH2Cl2
  8. dry with materialthe combined extracts dried over sodium sulfate
  9. concentrationconcentrated
  10. customto leave an oil

출처 및 근거

ORD 기록
ord-7919114cf47c4a468378cc435560f90a
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05077305

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트