Triethylamine → HCID 70207944、化合物

HRID 1378392ノート

反応式

HRID 1378392 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:16])=[C:11](F)[C:12]=3[F:14])[C:7](=[O:17])[C:6]([C:18]([OH:20])=[O:19])=[CH:5]2)[CH2:3][CH2:2]1.Cl.[OH:22][CH2:23][C@H:24]1[C@H:28]([C:29]([F:32])([F:31])[F:30])[CH2:27][NH:26][CH2:25]1.C(N(CC)CC)C>CS(C)=O>[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:16])=[C:11]([N:26]4[CH2:27][C@@H:28]([C:29]([F:31])([F:32])[F:30])[C@H:24]([CH2:23][OH:22])[CH2:25]4)[C:12]=3[F:14])[C:7](=[O:17])[C:6]([C:18]([OH:20])=[O:19])=[CH:5]2)[CH2:2][CH2:3]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 5354141-Cyclopropyl-6,7,8-trifluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acidHCID 70207387HCID 70207387、化合物

生成物 1

HCID 70207944HCID 70207944、化合物収率 95.4%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
50 °C

実験手順

In 6 ml of dimethylsulfoxide, is dissolved 283 mg (1 mmol) of 1-cyclopropyl-6,7,8-trifluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid. To the above solution, are added 411 mg (2 mmol) of trans-3-hydroxymethyl-4-trifluoromethylpyrrolidine hydrochloride and 0.42 ml (3 mmol) of triethylamine. The mixture is stirred at 50° C. for 18 hours. The reaction mixture was concentrated under reduced pressure. Water was added to the residue. The resulting precipitate was obtained by filtration and washed successively with water, isopropanol and diethyl ether to give 412 mg of the objective substance as a slightly yellow powder (yield 95.4%).

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionWater was added to the residue
  3. customThe resulting precipitate was obtained by filtration
  4. washwashed successively with water, isopropanol and diethyl ether

出典と根拠

ORDレコード
ord-f43c8a87b5f34869ab4f00226a0f6297
出典データセット
uspto-grants-1997_09
特許番号
US05668147

反応ノート

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