Triethylamine → 2-Nitrobenzyl perfluorooctanoate

HRID 1633182

反応式

HRID 1633182 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 150954062-Nitrobenzyl perfluorooctanoate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a285f827b3314d6696a0c8ee1e2afecb
出典データセット
uspto-grants-1984_10
特許番号
US04478967

関連ノート

読み込み中…