Triethylamine → HCID 13187387、化合物

HRID 434589

反応式

HRID 434589 の反応式
[NH:1]1[CH2:5][CH2:4][CH2:3][C:2]1=[O:6].C(N(CC)CC)C.[Cl:14][C:15]1[CH:33]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:31]=[CH:30][C:16]=1[O:17][C:18]1[CH:19]=[C:20]([C:24]([N+:27]([O-:29])=[O:28])=[CH:25][CH:26]=1)[C:21](Cl)=[O:22]>C1(C)C=CC=CC=1>[Cl:14][C:15]1[CH:33]=[C:32]([C:34]([F:35])([F:37])[F:36])[CH:31]=[CH:30][C:16]=1[O:17][C:18]1[CH:19]=[C:20]([C:24]([N+:27]([O-:29])=[O:28])=[CH:25][CH:26]=1)[C:21]([N:1]1[CH2:5][CH2:4][CH2:3][C:2]1=[O:6])=[O:22]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 120252-PyrrolidoneHCID 30177655-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chloride

生成物 1

HCID 13187387HCID 13187387、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

Pyrrolidin-2-one (7.60 grams; 0.02 mol), triethylamine (2.0 grams; 0.02 mol) and toluene (50 mol) were placed in a three-necked, glass reaction flask equipped with stirrer, thermometer, addition funnel and drying tube. 3-(2-Chloro-4-trifluoromethylphenoxy)-6-nitrobenzoylchloride (7.60 grams; 0.02 mol) in toluene (10 ml) was added to the mixture in the flask. The mixture, after being stirred overnight at room temperature, was washed with water, dried over sodium sulfate and evaporated to give a dark oil. The oil was chromatographed using silica gel into two fractions, the first using toluene as eluant and the second fraction using an equal mixture of toluene and ethyl acetate gave the desired product as a brown oil which solidified upon standing. Trituration with isopropyl ether resulted in white crystals, melting point 88° C. This product analyzed as follows:

後処理

  1. customglass reaction flask
  2. customequipped with stirrer
  3. additionthermometer, addition funnel
  4. customdrying tube
  5. washwas washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customto give a dark oil
  9. customThe oil was chromatographed
  10. additionan equal mixture of toluene and ethyl acetate

出典と根拠

ORDレコード
ord-f8e9e5573ba34c5085c7907967cd55bd
出典データセット
uspto-grants-1983_08
特許番号
US04398938

関連ノート

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