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2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 4-Acetyl-5-benzyloxy-2-(4benzyloxyphenyl)-1-ethylpyrrolo[2,1,5-cd]indolizine

HRID 1422096
ノート
印刷プレビュー

反応式

HRID 1422096 の反応式
[CH2:1]([O:8][C:9]1[CH:17]=[CH:16][C:15]2[N:11]([CH:12]=[C:13]([C:20]3[CH:25]=[CH:24][C:23]([O:26][CH2:27][C:28]4[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=4)=[CH:22][CH:21]=3)[C:14]=2[CH2:18][CH3:19])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:34][C:35](=[O:38])[C:36]#[CH:37].ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>C1(C)C=CC=CC=1>[C:35]([C:36]1[CH:37]=[C:12]2[N:11]3[C:15](=[CH:16][CH:17]=[C:9]([O:8][CH2:1][C:2]4[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=4)[C:10]=13)[C:14]([CH2:18][CH3:19])=[C:13]2[C:20]1[CH:21]=[CH:22][C:23]([O:26][CH2:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)=[CH:24][CH:25]=1)(=[O:38])[CH3:34]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 15018Butyn-2-oneHCID 187070166-Benzyloxy-2-(4-benzyloxyphenyl)-1-ethylindolizine

生成物 1

HCID 187070344-Acetyl-5-benzyloxy-2-(4benzyloxyphenyl)-1-ethylpyrrolo[2,1,5-cd]indolizine収率 38%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

6-Benzyloxy-2-(4-benzyloxyphenyl)-1-ehtylindolizine, prepared in example 23, step 5, (2.17 g, 5.0 mmol) was dissolved in 100 ml of dry toluene under a nitrogen atmosphere, and the mixture was stirred in an ice bath, while 3-butyn-2-one (0.34 ml, 5.75 mmol) was added dropwise. The cooling source was removed and stirring was continued for twenty hours. 2,3-Dichloro-5,6-dicyano-1,4-benzoquinone (0.57 g, 0.25 mmol) was added in portions and stirring was continued for 11/2 hour. The solvent was evaporated and the crude product was purified by column chromatography over silica gel 60, using 20% of ethyl acetate in petroleum ether as the eluent. Fractions containing the product were colleted and the solvent was evaporated. The crude product was and crystallized from diethyl ether to afford 0.955 g (38%) of 4-acetyl-5-benzyloxy-2-(4-benzyloxyphenyl)-1-ethylpyrrolo[2,1,5-cd]indolizine as crystals. MS(SP): m/z 499 (M+). 1H-NMR (CDCl3, 400 MHz) δ: 1.44 (t, 3H); 2.79 (s, 3H); 3.15 (q, 2H); 5.15 (s, 2H); 5.44 (s, 2H); 7.15 (d, 2H); 7.32-7.46 (m, 7H); 7.50 (d, 2H); 7.60 (d, 2H); 7.67-7.74 (m, 3H); 7.94 (s, 1H).

後処理

  1. additionwas added dropwise
  2. customThe cooling source was removed
  3. waitwas continued for twenty hours
  4. stirringstirring
  5. custom2 hour
  6. customThe solvent was evaporated
  7. customthe crude product was purified by column chromatography over silica gel 60
  8. additionFractions containing the product
  9. customthe solvent was evaporated
  10. customcrystallized from diethyl ether

出典と根拠

ORDレコード
ord-4b52fed64f604825b7c76e6812253b91
出典データセット
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06080754

反応ノート

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