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Sodium hydride → HCID 21476978、化合物

HRID 2293606
ノート
印刷プレビュー

反応式

HRID 2293606 の反応式
[C:1]([CH2:6][O:7][C:8]1[CH:41]=[C:40]([O:42][CH3:43])[CH:39]=[CH:38][C:9]=1[CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([O:20][CH2:21][CH2:22][CH3:23])=[CH:17][CH:18]=2)[C:13]([C:24]2[CH:29]=[CH:28][C:27]3[O:30][CH2:31][O:32][C:26]=3[CH:25]=2)=[C:12]1[C:33]([O:35]CC)=[O:34])([O:3]CC)=[O:2].C(COC1C=C(OC)C=CC=1CN1C2C(=CC(O)=CC=2)C(C2C=CC3OCOC=3C=2)=C1C(OCC)=O)(OCC)=O.[H-].[Na+].ICCC>CN(C=O)C>[C:1]([CH2:6][O:7][C:8]1[CH:41]=[C:40]([O:42][CH3:43])[CH:39]=[CH:38][C:9]=1[CH2:10][N:11]1[C:19]2[C:14](=[CH:15][C:16]([O:20][CH2:21][CH2:22][CH3:23])=[CH:17][CH:18]=2)[C:13]([C:24]2[CH:29]=[CH:28][C:27]3[O:30][CH2:31][O:32][C:26]=3[CH:25]=2)=[C:12]1[C:33]([OH:35])=[O:34])([OH:3])=[O:2]
参加物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 24758Sodium hydrideHCID 336431-IodopropaneHCID 21476971HCID 21476971、化合物HCID 21476972Ethyl 1-(2-carboethoxymethoxy-4-methoxybenzyl)-5-hydroxy-3-(3,4-methlenedioxyphenyl)indole-2-carboxylate

生成物 1

HCID 21476978HCID 21476978、化合物収率 47%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
2 回

実験手順

Ethyl 1-(2-Carboethoxymethoxy-4-methoxybenzyl)-3-(3,4-methlenedioxyphenyl)-5-(prop-1-yloxy)indole-2-carboxylate. To a solution of ethyl 1-(2-carboethoxymethoxy-4-methoxybenzyl)-5-hydroxy-3-(3,4-methylenedioxyphenyl)indole-2-carboxylate (175 mg, 0.30 mmol) in DMF stirred at ice bath temperature under an argon atmosphere was added a slurry of NaH (11 mg of 80% oil dispersion, 0.36 mmol, oil removed by pentane wash) in DMF (1 mL). After 15 min at ice bath temperature, 1-iodopropane (0.255 g, 1.5 mmol) was added and the ice bath was removed. The reaction mixture was stirred an additional 30 min at room temperature then partitioned between 3N HCl (25 mL) and EtOAc (75 mL). The organic extract was washed successively with H2O, aqueous NaHCO3, H2O and saturated aqueous NaCl and dried (Na2SO4). The solvent was removed in vacuo and the resulting solid crystallized from EtOH to afford the title compound (83 mg 47%); m.p. 89°-91° C.

後処理

  1. customthe ice bath was removed
  2. customthen partitioned between 3N HCl (25 mL) and EtOAc (75 mL)
  3. extractionThe organic extract
  4. washwas washed successively with H2O, aqueous NaHCO3, H2O and saturated aqueous NaCl
  5. dry with materialdried (Na2SO4)
  6. customThe solvent was removed in vacuo
  7. customthe resulting solid crystallized from EtOH

出典と根拠

ORDレコード
ord-2d3b872481914e04ba2687623c54f4d0
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05686481

反応ノート

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