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Triethylamine → HCID 20431439、化合物

HRID 1708858
ノート
印刷プレビュー

反応式

HRID 1708858 の反応式
[CH:1]([NH:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[CH2:2].ClCC=CC1C=CC=CC=1.C(N(CC)CC)C.[F:28][C:29]([F:48])([C:33]([F:47])([F:46])[C:34]([F:45])([F:44])[C:35]([F:43])([F:42])[C:36]([F:41])([F:40])[CH:37]([F:39])[F:38])[C:30](Cl)=[O:31]>C(C1C=CC=C(C(C)(C)C)C=1O)(C)(C)C.C(#N)C>[CH:1]([N:3]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[C:30](=[O:31])[C:29]([F:28])([F:48])[C:33]([F:46])([F:47])[C:34]([F:44])([F:45])[C:35]([F:42])([F:43])[C:36]([F:40])([F:41])[CH:37]([F:38])[F:39])=[CH2:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 94242Benzene, (3-chloro-1-propenyl)-HCID 27761327H-Perfluoroheptanoyl chlorideHCID 13751050Vinylbenzylamine

生成物 1

HCID 20431439HCID 20431439、化合物収率 65.2%

試薬・触媒・溶媒 2

HCID 31405
2,6-Di-tert-butylphenol
触媒
HCID 6342Acetonitrile溶媒

実験手順

300 ml of acetonitrile, 33.9 g (0.3 mol) of vinylbenzylamine (synthesized by the method described in "Kobunshi Gakkai Yokoshu", vol. 26, page 834 (G3 C-07) (1977) from chloromethylstyrene (meta:para=about 6:4); p.b.: 82° C./1.5 mm Hg), 30.3 g (0.3 mol) of triethylamine, and 0.5 g of 2,6-di-t-butylphenol were charged into a 500-ml three-necked flask equipped with a stirrer, and a calcium chloride tube, and the mixture was then cooled with ice water. 109.5 g (0.3 mol) of the 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoro-n-heptanoic acid chloride synthesized in Synthesis Example 1 was added dropwise, with stirring and ice-cooling. Next, the mixture was stirred for 1 hour at room temperature, and the deposited triethylamine hydrochloride was filtered off. The filtrate was distilled under reduced pressure to remove the acetonitrile, 200 ml of ethyl acetate was added to the remainder to be dissolved, and white insolubles were filtered off. The filtrate was distilled under reduced pressure to be condensed, and 300 ml of n-hexane was added to the remainder, followed by cooling. The deposited white crystals were filtered and dried in vacuo at room temperature, thus producing 90.1 g (yield: 65.2%; m.p.: 53° to 57° C.) of 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoro-n-heptanoic acid vinylbenzylamide.

後処理

  1. customequipped with a stirrer, and a calcium chloride tube
  2. additionwas added dropwise
  3. temperatureice-cooling
  4. stirringNext, the mixture was stirred for 1 hour at room temperature
  5. filtrationthe deposited triethylamine hydrochloride was filtered off
  6. distillationThe filtrate was distilled under reduced pressure
  7. customto remove the acetonitrile, 200 ml of ethyl acetate
  8. additionwas added to the remainder
  9. dissolutionto be dissolved
  10. filtrationwhite insolubles were filtered off
  11. distillationThe filtrate was distilled under reduced pressure
  12. customcondensed, and 300 ml of n-hexane
  13. additionwas added to the remainder
  14. temperatureby cooling
  15. filtrationThe deposited white crystals were filtered
  16. customdried in vacuo at room temperature

出典と根拠

ORDレコード
ord-f18de4123dd44e3ba715bad631854ee5
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04946771

反応ノート

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