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Diisopropyl Ether → Ethyl 2-[6-(3-amino-1-pyrrolidinyl)-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate

HRID 232466
ノート
印刷プレビュー

反応式

HRID 232466 の反応式
Cl[C:2]1[C:15]([F:16])=[CH:14][C:5]([C:6]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])=[C:4]([NH:17][C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=2[F:25])[N:3]=1.Cl.Cl.[NH2:28][CH:29]1[CH2:33][CH2:32][NH:31][CH2:30]1.C(N(CC)CC)C.C(OC(C)C)(C)C>C(Cl)(Cl)Cl.O>[NH2:28][CH:29]1[CH2:33][CH2:32][N:31]([C:2]2[C:15]([F:16])=[CH:14][C:5]([C:6]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])=[C:4]([NH:17][C:18]3[CH:23]=[CH:22][C:21]([F:24])=[CH:20][C:19]=3[F:25])[N:3]=2)[CH2:30]1
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 7914Diisopropyl EtherHCID 8471TriethylamineHCID 13849316Ethyl 2-[6-chloro-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetateHCID 162125963-Aminopyrrolidine dihydrochloride

生成物 1

HCID 13922528Ethyl 2-[6-(3-amino-1-pyrrolidinyl)-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate収率 84.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6212Chloroform溶媒2 回

実験手順

In 5 ml of chloroform was dissolved 500 mg of ethyl 2-[6-chloro-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate, and 260 mg of 3-aminopyrrolidine dihydrochloride and 500 mg of triethylamine were added thereto, after which the resulting mixture was subjected to reaction under reflux for 1.5 hours. Subsequently, the reaction mixture was added to a mixture of 5 ml of chloroform and 5 ml of water, and the organic layer was separated, washed successively with 5 ml of water and 5 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 2 ml of diisopropyl ether, after which crystals were collected by filtration to obtain 480 mg (yield 84.7%) of ethyl 2-[6-(3-amino-1-pyrrolidinyl)-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]acetate having a melting point of 140°-142° C.

後処理

  1. additionwere added
  2. customafter which the resulting mixture was subjected to reaction
  3. temperatureunder reflux for 1.5 hours
  4. customthe organic layer was separated
  5. washwashed successively with 5 ml of water and 5 ml of saturated aqueous sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under reduced pressure
  8. customto the crystalline material thus obtained
  9. filtrationafter which crystals were collected by filtration

出典と根拠

ORDレコード
ord-bdd635ee9df84c22a4182a4c426eb6b0
出典データセット
uspto-grants-1989_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04851535

反応ノート

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