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

Water → 2-[2-(Heptafluoropropoxy)-tetrafluoroethyl]-ethyl alcohol

HRID 132087
노트
인쇄 미리보기

반응식

HRID 132087 반응식
[C:1]([O:11][C:12]([C:15]([CH2:18][CH2:19]I)([F:17])[F:16])([F:14])[F:13])([C:4]([C:7]([F:10])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2].CNC=[O:24].O>CCOCC>[C:1]([O:11][C:12]([C:15]([CH2:18][CH2:19][OH:24])([F:17])[F:16])([F:14])[F:13])([C:4]([C:7]([F:10])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 31254N-MethylformamideHCID 87198538CF3CF2CF2Ocf2CF2CH2CH2I

생성물 1

HCID 577405752-[2-(Heptafluoropropoxy)-tetrafluoroethyl]-ethyl alcohol수율 85%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
150 °C

실험 절차

C3F7OCF2CF2I (100 g, 0.24 mol) and benzoyl peroxide (3 g) were charged under nitrogen into a vessel. A series of three vacuum/nitrogen gas sequences was then executed at −50° C. and ethylene (18 g, 0.64 mol) was introduced. The vessel was heated for 24 h at 110° C. The autoclave was cooled to 0° C. and opened after degassing. Then the product was collected in a bottle. The product was distilled to provide C3F7OCF2CF2CH2CH2I (80 g, 80% yield): bp 56-60° C. at 25 mm Hg (3325 Pa). A mixture of C3F7OCF2CF2CH2CH2I, (300 g, 0.68 mol) and N-methyl-formamide (300 mL), was heated to 150° C. for 26 h. Then the reaction was cooled to 100° C., followed by the addition of water to separate the crude ester. Ethyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester, and the reaction was stirred at 70° C. for 15 minutes. Then ethyl formate and ethyl alcohol were distilled out to give a crude product. The crude product was dissolved in ether, washed with aqueous sodium sulfite, water, and brine in turn, then dried over magnesium sulfate. The product was then distilled to provide C3F7OCF2CF2CH2CH2OH (B3, 199 g, 85% yield): bp 71˜73° C. at 40 mmHg (5320 Pa).

후처리

  1. temperatureThen the reaction was cooled to 100° C.
  2. customto separate the crude ester
  3. additionEthyl alcohol (77 mL) and p-toluene sulfonic acid (2.59 g) were added to the crude ester
  4. distillationThen ethyl formate and ethyl alcohol were distilled out
  5. customto give a crude product
  6. washwashed with aqueous sodium sulfite, water, and brine in turn
  7. dry with materialdried over magnesium sulfate
  8. distillationThe product was then distilled

출처 및 근거

ORD 기록
ord-cf9173b2ab574594a6ce9ad25b2c04a9
출처 데이터셋
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07385077B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트