Triethylamine → 2,3,4-Trifluorophenyl isothiocyanate

HRID 1085780ノート

反応式

HRID 1085780 の反応式
[C:1](Cl)(Cl)=[S:2].C(N(CC)CC)C.[F:12][C:13]1[C:19]([F:20])=[C:18]([F:21])[CH:17]=[CH:16][C:14]=1[NH2:15]>CCOCC>[F:12][C:13]1[C:19]([F:20])=[C:18]([F:21])[CH:17]=[CH:16][C:14]=1[N:15]=[C:1]=[S:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 774682,3,4-Trifluoroaniline

生成物 1

HCID 27607912,3,4-Trifluorophenyl isothiocyanate収率 77.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
20 °C

実験手順

Reference Example 1 Thiophosgene (1.4 g) was dissolved in 25 ml of ether, 2.0 g of triethylamine was added thereto with ice cooling and stirring (at not higher than 20° C.), then a mixture of 1.4 g of 2,3,4-trifluoroaniline and 3 ml of ether was gradually dropped thereinto at the same temperature, and the mixture was stirred for one hour at the same temperature. Then it was filtered off, the filtrate was concentrated, the residue was extracted with n-hexane, insoluble matters were removed by filtration, the resulting hexane-soluble matters were subjected to a silica gel column chromatography (Wacogel C-200 in the amount of 15 g) and eluted with n-hexane to give 1.39 g of 2,3,4-trifluorophenyl isothiocyanate.

後処理

  1. additionwas gradually dropped
  2. stirringat the same temperature, and the mixture was stirred for one hour at the same temperature
  3. filtrationThen it was filtered off
  4. concentrationthe filtrate was concentrated
  5. extractionthe residue was extracted with n-hexane, insoluble matters
  6. customwere removed by filtration
  7. washeluted with n-hexane

出典と根拠

ORDレコード
ord-69b2025f35364edb93d640fca35e61b8
出典データセット
uspto-grants-1991_04
特許番号
US05011831

反応ノート

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