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Potassium Carbonate → HCID 58505748、化合物

HRID 1917601
ノート
印刷プレビュー

反応式

HRID 1917601 の反応式
CC(C)(C)C(C1C(CC(C)(C)C(OCC)=O)=C(C(C2C=CC=CC=2)=O)N2C=1C=C(O)C=C2)=O.[Cl:34][C:35]1[CH:40]=[CH:39][C:38]([C:41]([C:43]2[N:51]3[C:46]([CH:47]=[C:48]([OH:52])[CH:49]=[CH:50]3)=[C:45]([C:53](=[O:58])[C:54]([CH3:57])([CH3:56])[CH3:55])[C:44]=2[CH2:59][C:60]([CH3:67])([CH3:66])[C:61]([O:63][CH2:64][CH3:65])=[O:62])=[O:42])=[CH:37][CH:36]=1.Cl.Cl[CH2:70][C:71]1[CH:80]=[CH:79][C:78]2[C:73](=[CH:74][CH:75]=[CH:76][CH:77]=2)[N:72]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:34][C:35]1[CH:36]=[CH:37][C:38]([C:41]([C:43]2[N:51]3[C:46]([CH:47]=[C:48]([O:52][CH2:70][C:71]4[CH:80]=[CH:79][C:78]5[C:73](=[CH:74][CH:75]=[CH:76][CH:77]=5)[N:72]=4)[CH:49]=[CH:50]3)=[C:45]([C:53](=[O:58])[C:54]([CH3:56])([CH3:57])[CH3:55])[C:44]=2[CH2:59][C:60]([CH3:66])([CH3:67])[C:61]([O:63][CH2:64][CH3:65])=[O:62])=[O:42])=[CH:39][CH:40]=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 11430Potassium CarbonateHCID 30838232-(Chloromethyl)quinoline hydrochlorideHCID 178471306HCID 178471306、化合物HCID 178471307HCID 178471307、化合物

生成物 1

HCID 58505748HCID 58505748、化合物

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
23 °C

実験手順

To a stirred solution of ethyl 3-[7-(benzyloxy)-3-[(4-chlorophenyl)carbonyl]-1-(2,2-dimethylpropanoyl)indolizin-2-yl]-2,2-dimethylpropanoate (3.50 g, 6.10 mmol) in EtOH (50 mL) is added 10% Pd/C (480 mg). The suspension is stirred under an atmosphere of hydrogen for 1.5 h then filtered through a pad of diatomaceous earth and washed with EtOH. The filtrate is concentrated in vacuo to give ethyl 3-{3-[(4-chlorophenyl)carbonyl]-1-(2,2-dimethylpropanoyl)-7-hydroxyindolizin-2-yl}-2,2-dimethylpropanoate (2.50 g, 85%). Also obtained is ethyl 3-[1-(2,2-dimethylpropanoyl)-7-hydroxy-3-(phenylcarbonyl)indolizin-2-yl]-2,2-dimethylpropanoate (0.28 g, 10%). A suspension of ethyl 3-{3-[(4-chlorophenyl)carbonyl]-1-(2,2-dimethylpropanoyl)-7-hydroxyindolizin-2-yl}-2,2-dimethylpropanoate (100 mg, 0.207 mmol), 2-(chloromethyl)quinoline-HCl (66.0 mg, 0.310 mmol), and potassium carbonate (114 mg, 0.826 mmol) in DMF (3 mL) is stirred for 24 h at 23° C. The mixture is filtered and concentrated in vacuo to give ethyl 3-{3-[(4-chlorophenyl)carbonyl]-1-(2,2-dimethylpropanoyl)-7-(quinolin-2-ylmethoxy)indolizin-2-yl}-2,2-dimethylpropanoate that is dissolved in THF (2 mL), MeOH (3 mL), and 6M aqueous NaOH (2 mL) and heated at 70° C. for 1 h then cooled to 23° C. and acidified to pH=1 with concentrated aqueous HCl. The mixture is partitioned between CH2Cl2 and brine then organics are dried with MgSO4, filtered, and concentrated in vacuo. Purification of the crude by HPLC (25 to 75% CH3CN/0.1% TFA in water) gives the title compound (60 mg, 49%).

後処理

  1. customAlso obtained
  2. filtrationThe mixture is filtered
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9f658869ca4440bc84283d9b85939d9d
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08618300B2

反応ノート

読み込み中…

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