Triethylamine → 2-Nitrobenzyl perfluorooctanoate

HRID 1633182

반응식

HRID 1633182 반응식
[F:1][C:2]([F:25])([C:6]([F:24])([F:23])[C:7]([F:22])([F:21])[C:8]([F:20])([F:19])[C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[C:3](Cl)=[O:4].[N+:26]([C:29]1[CH:36]=[CH:35][CH:34]=[CH:33][C:30]=1[CH2:31][OH:32])([O-:28])=[O:27].C(N(CC)CC)C.Cl.C(N(CC)CC)C>C1C=CC=CC=1>[F:1][C:2]([F:25])([C:6]([F:24])([F:23])[C:7]([F:22])([F:21])[C:8]([F:20])([F:19])[C:9]([F:18])([F:17])[C:10]([F:16])([F:15])[C:11]([F:14])([F:13])[F:12])[C:3]([O:32][CH2:31][C:30]1[CH:33]=[CH:34][CH:35]=[CH:36][C:29]=1[N+:26]([O-:28])=[O:27])=[O:4]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 11130Triethylamine hydrochlorideHCID 119232-Nitrobenzyl alcoholHCID 78978Perfluorooctanoyl chloride

생성물 1

HCID 150954062-Nitrobenzyl perfluorooctanoate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

Perfluorooctanoyl chloride (21.6 g, 0.05 mol) was added slowly with stirring to a solution of 2-nitrobenzyl alcohol (7.65 g, 0.05 mol) and triethylamine (5.2 g, 0.05 mol) in 100 ml benzene. During the addition, the temperature was allowed to rise to 50° C. and the triethylamine hydrochloride began to precipitate. After the addition was complete, the reaction was stirred an additional 30 minutes. The reaction was filtered and the filtrate evaporated in vacuo to give an oil which crystallized on cooling in an ice bath (m.p. 34°-35° C.). Benzene washings of the material retained on the filter paper gave a second fraction of oil which crystallized on cooling. Total yield was 11.97 g.

후처리

  1. additionDuring the addition
  2. customto rise to 50° C.
  3. customto precipitate
  4. additionAfter the addition
  5. filtrationThe reaction was filtered
  6. customthe filtrate evaporated in vacuo
  7. customto give an oil which
  8. customcrystallized
  9. temperatureon cooling in an ice bath (m.p. 34°-35° C.)
  10. customgave a second fraction of oil which
  11. customcrystallized
  12. temperatureon cooling

출처 및 근거

ORD 기록
ord-a285f827b3314d6696a0c8ee1e2afecb
출처 데이터셋
uspto-grants-1984_10
특허 번호
US04478967

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