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Z-6-chloro-3-(3-chloro-benzylidene)-1,3-dihydro-indol-2-one → 6-ethoxy-spiro[cyclohexane-1,3'-[3H]indole]-2',4(1'H)-dione

HRID 1987803
ノート
印刷プレビュー

反応式

HRID 1987803 の反応式
Cl[C:2]1[CH:10]=[C:9]2[C:5](/[C:6](=[CH:12]/C3C=CC=C(Cl)C=3)/[C:7](=[O:11])[NH:8]2)=[CH:4][CH:3]=1.[CH2:20]([O:22][CH:23]=[CH:24][C:25](=[CH2:31])[O:26][Si](C)(C)C)[CH3:21]>C1(C)C=CC=CC=1>[CH2:20]([O:22][CH:23]1[C:6]2([C:5]3[C:9](=[CH:10][CH:2]=[CH:3][CH:4]=3)[NH:8][C:7]2=[O:11])[CH2:12][CH2:26][C:25](=[O:31])[CH2:24]1)[CH3:21]
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

4

反応物 2

HCID 57507271Z-6-chloro-3-(3-chloro-benzylidene)-1,3-dihydro-indol-2-oneHCID 85441339(3-Ethoxy-1-methylene-allyloxy)-trimethyl-silane

生成物 1

HCID 867608916-ethoxy-spiro[cyclohexane-1,3'-[3H]indole]-2',4(1'H)-dione収率 23.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
140 °C

実験手順

To a suspension of E/Z-6-chloro-3-(3-chloro-benzylidene)-1,3-dihydro-indol-2-one (1.45 g, 15.0 mmol) in toluene (20 mL) in a sealed tube was added (3-ethoxy-1-methylene-allyloxy)-trimethyl-silane (1.24 g, 7.5 mmol). The reaction mixture was allowed to stir at 140° C. for 16 hrs. The solvent was removed by concentration. The residue was dissolved in MeOH (50 mL) and treated with 4 N NaOH (5 mL) at rt for 0.5 h. The reaction mixture was then diluted with AcOEt and washed with water and brine. After concentration the residue was purified by flash column (5%-30% AcOEt in Hex) to give a mixture (1.2 g) of rac-(1R,2R)-6′-chloro-2-(3-chlorophenyl)spiro[5-cyclohexene-1,3′-[3H]indole]-2′,4(1′H)-dione and rac-(1R,2S,6R)-6′-chloro-2-3-chlorophenyl)-6-ethoxy-spiro[cyclohexane-1,3′-[3H]indole]-2′,4(1′H)-dione (0.46 g, 18.6%) as white amorphous which was used for next steps without further purification. A small amount mixture was separated by normal phase HPLC gave rac-(1R,2S,6R)-6′-chloro-2-(3-chlorophenyl)-6-ethoxy-spiro[cyclohexane-1,3′-[3H]indole]-2′,4(1′H)-dione. MS+:358 (M+1).

後処理

  1. customThe solvent was removed by concentration
  2. dissolutionThe residue was dissolved in MeOH (50 mL)
  3. additiontreated with 4 N NaOH (5 mL) at rt for 0.5 h
  4. additionThe reaction mixture was then diluted with AcOEt
  5. washwashed with water and brine
  6. concentrationAfter concentration the residue
  7. customwas purified by flash column (5%-30% AcOEt in Hex)

出典と根拠

ORDレコード
ord-1473a77e4acc4f3faf38121d732dc94a
出典データセット
uspto-grants-2009_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07553833B2

反応ノート

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