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Phosgene → WAY127093B racemate

HRID 1612945
ノート
印刷プレビュー

反応式

HRID 1612945 の反応式
[C:1](Cl)(Cl)=[O:2].C(N(CC)CC)C.[N:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][NH2:19])[CH:13]=1.[CH:20]1([O:25][C:26]2[CH:27]=[C:28]([CH:34]3[N:38]([CH3:39])[NH:37][C:36](=[O:40])[CH2:35]3)[CH:29]=[CH:30][C:31]=2[O:32][CH3:33])[CH2:24][CH2:23][CH2:22][CH2:21]1>O1CCCC1>[CH:20]1([O:25][C:26]2[CH:27]=[C:28]([CH:34]3[CH2:35][C:36](=[O:40])[N:37]([C:1]([NH:19][CH2:18][C:14]4[CH:13]=[N:12][CH:17]=[CH:16][CH:15]=4)=[O:2])[N:38]3[CH3:39])[CH:29]=[CH:30][C:31]=2[O:32][CH3:33])[CH2:21][CH2:22][CH2:23][CH2:24]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 4

HCID 6371PhosgeneHCID 8471Triethylamine2 回HCID 310183-PyridinemethanamineHCID 197927655-[3-(Cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

生成物 1

HCID 19792796WAY127093B racemate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
-15 °C

実験手順

To a -15° C. solution of phosgene (4.50 mmol, 2.30 mL; 1.9M solution in toluene) in dry tetrahydrofuran (8 mL) is added neat triethylamine (4.50 mmol, 0.450 g; 0.620 mL) and the resulting suspension is stirred at -15° C. for 10 minutes. To this suspension is added 3-picolylamine (4.50 mmol, 0.490 g; 0.460 mL) and triethylamine (4.50 mmol, 0.450 g; 0.620 mL) in dry tetrahydrofuran (10 mL) in one portion and the reaction mixture is stirred at -15° C. for 30 minutes. Subsequently, 5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone (3.0 mmol, 0.870 g) in dry tetrahydrofuran (7 mL) is added at -15° C. and the reaction mixture is allowed to warm to room temperature overnight. The reaction is quenched with water (20 mL), the volatiles removed in vacuo, and the residue partitioned between ethyl acetate (150 mL) and water (150 mL). The organic layer is dried (Na2SO4) and concentrated in vacuo to give a tan solid. This material is purified by flash chromatography (SiO2 :1) 50% ethyl acetate/hexane; 2) 100% ethyl acetate; 3) 5% methanol/ethyl acetate) to give a mixture of starting material and product which is triturated with ether. The title compound is isolated as a white solid (0.158 g; 12%). Also isolated is a mixture of starting pyridazone and title compound (0.511 g). 1H-NMR (DMSO-d6, 400 MHz) δ8.45 (m, 3H); 7.65 (dt, 1H, J=8.0, 1.6 Hz); 7.22 (ddd, 1H, J=8.0, 5.0, 0.7 Hz); 6.94 (d, 1H, J=2.0 Hz); 6.88 (d, 1H, J=8.0 Hz); 6.82 (dd, 1H, J=8.0, 2.0 Hz); 4.63 (m, 1H); 4.38 (m, 3H); 3.70 (s, 3H); 3.65 (m, 1H); 2.74 (s, 3H); 2.65 (m, 1H); 1.79 (m, 2H); 1.63 (m, 4H); 1.49 (m, 2H). IR (KBr, cm-1) 3420, 3320, 2950, 1730, 1715, 1530, 1515, 1235, 1135.

後処理

  1. stirringthe reaction mixture is stirred at -15° C. for 30 minutes
  2. temperatureto warm to room temperature overnight
  3. customThe reaction is quenched with water (20 mL)
  4. customthe volatiles removed in vacuo
  5. customthe residue partitioned between ethyl acetate (150 mL) and water (150 mL)
  6. dry with materialThe organic layer is dried (Na2SO4)
  7. concentrationconcentrated in vacuo
  8. customto give a tan solid
  9. customThis material is purified by flash chromatography (SiO2 :1) 50% ethyl acetate/hexane
  10. custom3) 5% methanol/ethyl acetate) to give
  11. additiona mixture of starting material and product which
  12. customis triturated with ether

出典と根拠

ORDレコード
ord-b2e0ff8677dd47e6bf9d4c5d9b5902ee
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05191084

反応ノート

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