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

Triethylamine → Methyl 4-[(diethoxyphosphinyl)oxy]-2,6-bis(trifluoromethyl)-3-pyridinecarboxylate

HRID 542113
노트
인쇄 미리보기

반응식

HRID 542113 반응식
C(N(CC)CC)C.[P:8]([O-:15])([O:12][CH2:13][CH3:14])[O:9][CH2:10][CH3:11].[F:16][C:17]([F:34])([F:33])[C:18]1[C:23]([C:24]([O:26][CH3:27])=[O:25])=[C:22]([OH:28])[CH:21]=[C:20]([C:29]([F:32])([F:31])[F:30])[N:19]=1>C(Cl)(Cl)(Cl)Cl>[CH2:10]([O:9][P:8]([O:12][CH2:13][CH3:14])([O:28][C:22]1[CH:21]=[C:20]([C:29]([F:32])([F:31])[F:30])[N:19]=[C:18]([C:17]([F:33])([F:16])[F:34])[C:23]=1[C:24]([O:26][CH3:27])=[O:25])=[O:15])[CH3:11]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 3780918DiethylphosphiteHCID 178498966Methyl 2,6-bis(trifluoromethyl)-4-hydroxy-3-pyridinecarboxylate

생성물 1

HCID 13882876Methyl 4-[(diethoxyphosphinyl)oxy]-2,6-bis(trifluoromethyl)-3-pyridinecarboxylate수율 82%

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매

반응 조건

온도
0 °C

실험 절차

Triethylamine (25.2 ml, 0.18 mol) was added dropwise to a cooled (0° C.) solution of diethyl phosphite (23.2 ml, 0.18 mol) and product of Example 4 (50.0 g, 0.17 mol) in carbon tetrachloride (100 ml). The reaction mixture, which had developed a heavy flocculent precipitate, was stirred at 0° C. for 30 minutes before being warmed to room temperature for an additional 24 hours. The reaction mixture was washed consecutively with 1N aq hydrochloric acid (1×250 ml), 0.5N aqueous sodium hydroxide (4×100 ml) and water (1×250 ml) before being dried (MgSO4), filtered and evaporated (aspirator) to a yellow oil (61.53 g). Kugelrohr distillation (120° C. at 25 Pa) afforded the product as a very pale yellow oil (59.03 g). Yield-82%, nD25 1.4197.

후처리

  1. temperaturebefore being warmed to room temperature for an additional 24 hours
  2. washThe reaction mixture was washed consecutively with 1N aq hydrochloric acid (1×250 ml), 0.5N aqueous sodium hydroxide (4×100 ml) and water (1×250 ml)
  3. dry with materialbefore being dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated (aspirator) to a yellow oil (61.53 g)
  6. distillationKugelrohr distillation (120° C. at 25 Pa)

출처 및 근거

ORD 기록
ord-64db6b6c6f2c43699977f89470a61480
출처 데이터셋
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04655816

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트