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Iodine → ethyl [(1RS,2RS)-6-methoxy-2-p-methoxyphenyl-1,2,3,4-tetrahydronaphth-1-yl]acetate

HRID 1200090
ノート
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反応式

HRID 1200090 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[CH:8]([C:14]1[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=1)[CH2:7][CH2:6]2.Br[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].II.[Cl-].[NH4+]>[Zn].C1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[CH:9]([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH:8]([C:14]1[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=1)[CH2:7][CH2:6]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 807IodineHCID 7748Ethyl bromoacetateHCID 25517Ammonium ChlorideHCID 134065432-(4-Methoxyphenyl)-6-methoxy-1-tetralone

生成物 1

HCID 19861943ethyl [(1RS,2RS)-6-methoxy-2-p-methoxyphenyl-1,2,3,4-tetrahydronaphth-1-yl]acetate

試薬・触媒・溶媒 2

HCID 23994Zinc触媒
HCID 241Benzene溶媒

実験手順

A stirred mixture of 3,4-dihydro-6-methoxy-2-p-methoxyphenylnaphthalen-1(2H)-one (10 g.), ethyl bromoacetate (17.8 g.), zinc (11.6 g.), benzene (200 ml.) and one crystal of iodine was heated under reflux under an atomsphere of argon for 10 minutes, allowed to continue to boil until the exothermic reaction subsided, heated again under reflux for a further 10 minutes and then cooled to laboratory temperature. Saturated aqueous ammonium chloride solution (100 ml.) was added, the mixture was filtered and the organic layer of the filtrate was separated, dried and evaporated to dryness. A 10% palladium-on-charcoal catalyst (2 g.) was added to a solution of the residue (13.1 g.) in ethyl acetate (300 ml.) and the mixture was stirred under an atmosphere of hydrogen for 3 hours, filtered, and rehydrogenated with fresh catalyst (2 g.) for 18 hours. The mixture was filtered, the filtrate was evaporated to dryness and the residue was purified by chromatography on a silica gel column using a 25:1 v/v mixture of toluene and ethyl acetate. The ethyl [(1RS,2RS)-6-methoxy-2-p-methoxyphenyl-1,2,3,4-tetrahydronaphth-1-yl]acetate thus obtained was reduced with lithium aluminium hydride (4.4 g.) by a similar process to that described in Example 7, and the ethanol thus obtained (m.p. 98°-99° C.) was oxidised with pyridinium chlorochromate (8.6 g.) by a similar process to that described in the 6th paragraph of Example 2. There was thus obtained the desired acetaldehyde, m.p. 101°-103° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux under an atomsphere of argon for 10 minutes
  3. customto boil until the exothermic reaction
  4. temperatureheated again
  5. temperatureunder reflux for a further 10 minutes
  6. temperaturecooled to laboratory temperature
  7. filtrationthe mixture was filtered
  8. customthe organic layer of the filtrate was separated
  9. customdried
  10. customevaporated to dryness
  11. additionA 10% palladium-on-charcoal catalyst (2 g.) was added to a solution of the residue (13.1 g.) in ethyl acetate (300 ml.)
  12. filtrationfiltered
  13. waitrehydrogenated with fresh catalyst (2 g.) for 18 hours
  14. filtrationThe mixture was filtered
  15. customthe filtrate was evaporated to dryness
  16. customthe residue was purified by chromatography on a silica gel column
  17. additiona 25:1 v/v mixture of toluene and ethyl acetate

出典と根拠

ORDレコード
ord-d159605e2f4848bd935f8372a08fbaac
出典データセット
uspto-grants-1990_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04904661

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