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Hydrochloric Acid → [1R*,8S*,9aR*]1-Carbomethoxy-5,6-dimethoxy-8-phenyl-2,3,7,8,9,9a-hexahydrophenalene

HRID 1089026
ノート
印刷プレビュー

反応式

HRID 1089026 の反応式
[C:1]([C@@H:5]1[C@@H:16]2[C:17]3[C:8](=[CH:9][C:10]([O:26][CH3:27])=[C:11]([O:24][CH3:25])[C:12]=3[CH2:13][C@@H:14]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:15]2)[C:7](O)=[CH:6]1)([O:3][CH3:4])=[O:2].C(OCC)(=O)C.Cl.[H][H]>CO.[Pd]>[C:1]([C@H:5]1[C@@H:16]2[C:17]3[C:8](=[CH:9][C:10]([O:26][CH3:27])=[C:11]([O:24][CH3:25])[C:12]=3[CH2:13][C@@H:14]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)[CH2:15]2)[CH2:7][CH2:6]1)([O:3][CH3:4])=[O: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 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 70053121HCID 70053121、化合物HCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 18641660[1R*,8S*,9aR*]1-Carbomethoxy-5,6-dimethoxy-8-phenyl-2,3,7,8,9,9a-hexahydrophenalene

試薬・触媒・溶媒 2

HCID 23938
Palladium
触媒
HCID 887Methanol溶媒

実験手順

To a solution of 0.5 g (1.3 mmol) of [1R,8S,9aR]-1-carbomethoxy 5,6 dimethoxy 3 hydroxy 8 phenyl-7,8,9,9a-tetrahydro-phenalene (54-3A), in 50 mL of methanol, 50 mL of ethyl acetate and 0.1 mL of concentrated aqueous hydrochloric acid was added 0.2 g of 5% palladium on carbon and the reaction mixture was shaken under 4 atmospheres of hydrogen until the uptake of hydrogen had ceased. The palladium catalyst was removed by filtration through Celite filter aid and the filtrate was concentrated to give a white solid, which was carried on to the next step without purification.

後処理

  1. customThe palladium catalyst was removed by filtration through Celite
  2. filtrationfilter aid
  3. concentrationthe filtrate was concentrated
  4. customto give a white solid, which
  5. customwas carried on to the next step without purification

出典と根拠

ORDレコード
ord-f3418961b542490b810f81205f3b39a0
出典データセット
uspto-grants-1990_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04963568

反応ノート

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