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Pyrrolidone carboxylic acid → HCID 58477259、化合物

HRID 876528
ノート
印刷プレビュー

反応式

HRID 876528 の反応式
S(Cl)(Cl)=O.[O:5]=[C:6]1[NH:10][CH:9]([C:11]([OH:13])=O)[CH2:8][CH2:7]1.[NH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[C:19]2[C:24]=1[O:23][C:22]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[C:31]([F:34])([F:33])[F:32])=[CH:21][C:20]2=[O:35].N1C=CC=CC=1>C1COCC1.CN(C=O)C>[O:5]=[C:6]1[NH:10][CH:9]([C:11]([NH:14][C:15]2[CH:16]=[CH:17][CH:18]=[C:19]3[C:24]=2[O:23][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[C:31]([F:34])([F:32])[F:33])=[CH:21][C:20]3=[O:35])=[O:13])[CH2:8][CH2:7]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 499Pyrrolidone carboxylic acidHCID 1049PyridineHCID 24386Thionyl ChlorideHCID 58477328HCID 58477328、化合物

生成物 1

HCID 58477259HCID 58477259、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

Thionylchloride (236 mg, 2.0 mmol) was added to a solution of 5-oxopyrrolidine-2-carboxylic acid 120 (170 mg, 1.32 mmol) in THF (5 mL) at 0° C. DMF (1 drop) was added and the solution was allowed to warm to room temperature for 2 h then cooled to 0° C. A solution of 8-amino-2-(2-(trifluoromethyl)phenyl)-4H-chromen-4-one 11 (100 mg, 0.33 mmol) and pyridine (0.5 mL) in THF (1 mL) was added and the reaction mixture was allowed to warm to room temperature and stirred for 2 h. The reaction mixture was concentrated to dryness, dissolved in EtOAc, washed with sat. aq NaHCO3, brine, and dried (Na2SO4). The crude residue was purified by preparative TLC eluting with EtOAc to give Compound 313. MS (ESI) calcd for C21H15F3N2O4: 416.1. found: 417 [M+H].

後処理

  1. temperaturethen cooled to 0° C
  2. temperatureto warm to room temperature
  3. concentrationThe reaction mixture was concentrated to dryness
  4. dissolutiondissolved in EtOAc
  5. washwashed with sat. aq NaHCO3, brine
  6. dry with materialdried (Na2SO4)
  7. customThe crude residue was purified by preparative TLC
  8. washeluting with EtOAc

出典と根拠

ORDレコード
ord-6537d3f51e2a4868b9937490996ea6bd
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987258B2

反応ノート

読み込み中…

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