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Hydrochloric Acid → 2-(Propenyl)-5-[4-(4-propylcyclohexyl)phenyl]selenophene

HRID 1873389
ノート
印刷プレビュー

反応式

HRID 1873389 の反応式
[CH3:1][C:2](C)([O-])C.[K+].[CH2:7]([CH:10]1[CH2:15][CH2:14][CH:13]([C:16]2[CH:21]=[CH:20][C:19]([C:22]3[Se:26][C:25]([CH:27]=O)=[CH:24][CH:23]=3)=[CH:18][CH:17]=2)[CH2:12][CH2:11]1)[CH2:8][CH3:9].Cl>[Br-].C([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)C.C1COCC1.CC(OC)(C)C.[Cl-].[NH4+]>[CH:27]([C:25]1[Se:26][C:22]([C:19]2[CH:20]=[CH:21][C:16]([CH:13]3[CH2:14][CH2:15][CH:10]([CH2:7][CH2:8][CH3:9])[CH2:11][CH2:12]3)=[CH:17][CH:18]=2)=[CH:23][CH:24]=1)=[CH:1][CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 313Hydrochloric AcidHCID 23665647Potassium tert-butoxideHCID 594562815-[4-(4-Propylcyclohexyl)phenyl]selenophene-2-carbaldehyde

生成物 1

HCID 722902572-(Propenyl)-5-[4-(4-propylcyclohexyl)phenyl]selenophene

試薬・触媒・溶媒 4

HCID 73727Phosphonium, ethyltriphenyl-, bromide (1:1)触媒
HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 15413tert-Butyl methyl ether溶媒
HCID 25517Ammonium Chloride溶媒

実験手順

1.80 g (4.85 mmol) of ethyltriphenylphosphonium bromide are initially introduced in 8 ml of THF at 0° C., and 533 mg (4.75 mmol) of potassium tert-butoxide are added. After 1.5 h at RT, a solution of 1.16 g (3.23 mmol) of 5-[4-(4-propylcyclohexyl)phenyl]selenophene-2-carbaldehyde in 7 ml of THF is added, and the batch is stirred for 2.5 h. The mixture is diluted with MTBE, and sat. ammonium chloride soln. and 2 N hydrochloric acid are added. The organic phase is separated off, and the aqueous phase is extracted with MTBE. The combined organic phases are washed with sat. sodium chloride soln. and dried using sodium sulfate. The solution is concentrated to dryness, and the residue is purified by column chromatography (SiO2, n-heptane→n-heptane:EtOAc=20:1). 2-(Propenyl)-5-[4-(4-propylcyclohexyl)phenyl]selenophene is obtained as an E/Z isomer mixture.

後処理

  1. customThe organic phase is separated off
  2. extractionthe aqueous phase is extracted with MTBE
  3. washThe combined organic phases are washed with sat. sodium chloride soln
  4. customand dried
  5. concentrationThe solution is concentrated to dryness
  6. customthe residue is purified by column chromatography (SiO2, n-heptane→n-heptane:EtOAc=20:1)

出典と根拠

ORDレコード
ord-d5bb2c20a2c24e3886367c461b81c583
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08304036B2

反応ノート

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