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Dichloromethane → HCID 19774607、化合物

HRID 1613922
ノート
印刷プレビュー

反応式

HRID 1613922 の反応式
C[O-].[Na+].O=[C:5]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH2:6][CH2:7][CH:8]=O.[CH:17]1[CH2:21][CH:20]=[CH:19][CH:18]=1.C(Cl)Cl>CO>[CH2:10]([C:5]1[CH:6]=[CH:7][CH:8]=[C:17]2[C:18]=1[CH:19]=[CH:20][CH2:21]2)[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]
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 6344DichloromethaneHCID 7612CyclopentadieneHCID 10942334Sodium MethoxideHCID 131934644-Oxoundecanal

生成物 1

HCID 19774607HCID 19774607、化合物収率 34%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

20.4 ml of a 30 percent strength solution of sodium methanolate (111 mmol) in methanol were initially introduced into the reaction vessel at 0° C., and a mixture of 9.0 g (44.5 mmol) of 4-oxoundecylaldehyde and 4.0 ml (49 mmol) of cyclopentadiene was added in the course of 30 minutes. After the mixture had been stirred at 0° C. for 2 hours and at room temperature for a further 3 hours, it was hydrolyzed, methylene chloride was added and the mixture was filtered over Corolite. The organic phase was separated off, dried over MgSO4 and evaporated. Column chromatography with hexane as the mobile phase gave 3.2 g (34%) of the indene 17. For the NMR data, see Table 1.

後処理

  1. additionwas added in the course of 30 minutes
  2. filtrationthe mixture was filtered over Corolite
  3. customThe organic phase was separated off
  4. dry with materialdried over MgSO4
  5. customevaporated

出典と根拠

ORDレコード
ord-8f00b088d2f34ca3baa014eb7cc85157
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05194619

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート