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Phosgene → 3-[3-(cyclopentyloxy)-4-methoxyphenyl]-2,5-dihydro-2-methyl-5-oxo-1H-pyrazole-1-carboxamide

HRID 1655627
ノート
印刷プレビュー

反応式

HRID 1655627 の反応式
[C:1](Cl)(Cl)=[O:2].[CH:5]1([O:10][C:11]2[CH:12]=[C:13]([C:19]3[N:23]([CH3:24])[NH:22][C:21](=[O:25])[CH:20]=3)[CH:14]=[CH:15][C:16]=2[O:17][CH3:18])[CH2:9][CH2:8][CH2:7][CH2:6]1.C[Si](C)(C)[NH:28][Si](C)(C)C>O1CCCC1.O1C=CC=C1.O1CCCC1>[CH:5]1([O:10][C:11]2[CH:12]=[C:13]([C:19]3[N:23]([CH3:24])[N:22]([C:1]([NH2:28])=[O:2])[C:21](=[O:25])[CH:20]=3)[CH:14]=[CH:15][C:16]=2[O:17][CH3:18])[CH2:6][CH2:7][CH2:8][CH2:9]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6371PhosgeneHCID 13838HexamethyldisilazaneHCID 197927825-[3-(cyclopentyloxy)-4-methoxyphenyl]-1,2-dihydro-1-methyl-3H-pyrazol-3-one

生成物 1

HCID 197927913-[3-(cyclopentyloxy)-4-methoxyphenyl]-2,5-dihydro-2-methyl-5-oxo-1H-pyrazole-1-carboxamide収率 78%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 22709418Tetrahydrofuran furan溶媒

反応条件

温度
0 °C

実験手順

To a 0° C. solution of phosgene (8.75 mmol, 4.61 mL; 1.9 M solution in toluene) in dry tetrahydrofuran (30 mi) is added 5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1,2-dihydro-1-methyl-3H-pyrazol-3-one (7.0 mmol, 2.02 g) in dry tetrahydrofuran furan (15 mL) dropwise over 20 minutes. The resulting cloudy solution is stirred at 0° C. for 10 minutes and at room temperature for 1 hour after which a homogenous solution is obtained. The reaction mixture is cooled to 0° C. and hexamethyldisilazane (17.5 mmol, 2.82 g; 3.64 mi) in dry tetrahydrofuran (15 mL) is added in one portion. The resulting suspension is stirred at room temperature for 1 hour and then the volatiles are removed in vacuo. The residue is partitioned between 2% aqueous acetic acid (200 mi) and ethyl acetate (200 mi) and the aqueous phase is extracted with ethyl acetate (150 mL). The combined organic layers are washed with H2O (100 mL), dried (Na2SO4), and concentrated in vacuo to afford a tan solid. This material is triturated with ether and dried in vacuo for 1 hour at 60° C. to give the title compound as a white solid (1.80 g; 78%). 1H NMR (DMSO-d6 400 MHz) δ 7.23 (br s, 1H); 7.02 (m, 3H); 6.92 (br s, 1H); 6.08 (s, 1H); 4.86 (m, 1H); 3.78 (s, 3H); 3.72 (s, 3H); 1.88 (m, 2H); 1.70 (m, 4H); 1.56 (m, 2H). IR (KBr, cm-1) 3400, 3300, 3200, 2950, 1760, 1500,1330,1250,1130.

後処理

  1. customis obtained
  2. temperatureThe reaction mixture is cooled to 0° C.
  3. stirringThe resulting suspension is stirred at room temperature for 1 hour
  4. customthe volatiles are removed in vacuo
  5. customThe residue is partitioned between 2% aqueous acetic acid (200 mi) and ethyl acetate (200 mi)
  6. extractionthe aqueous phase is extracted with ethyl acetate (150 mL)
  7. washThe combined organic layers are washed with H2O (100 mL)
  8. dry with materialdried (Na2SO4)
  9. concentrationconcentrated in vacuo
  10. customto afford a tan solid
  11. customThis material is triturated with ether
  12. customdried in vacuo for 1 hour at 60° C.

出典と根拠

ORDレコード
ord-2379be1d94854a009dfa63efd244cc5a
出典データセット
uspto-grants-1993_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05250700

反応ノート

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