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Tetrahydrofuran → 1,5-Bis-(4-benzyloxy-3-methoxy-phenyl)-pentan-3-one

HRID 356457
ノート
印刷プレビュー

反応式

HRID 356457 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[CH:16][C:17](=[O:36])[CH:18]=[CH:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][CH2:27][C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)=[C:22]([O:34][CH3:35])[CH:21]=2)=[CH:11][C:10]=1[O:37][CH3:38])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[O-]S([O-])(=O)=O.[Ba+2].C1COCC1.CC(C)=O.OS(O)(=O)=O.O=[Cr](=O)=O>CC(C)=O.[Pd].C(O)(C)C>[CH2:27]([O:26][C:23]1[CH:24]=[CH:25][C:20]([CH2:19][CH2:18][C:17](=[O:36])[CH2:16][CH2:15][C:12]2[CH:13]=[CH:14][C:9]([O:8][CH2:1][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=3)=[C:10]([O:37][CH3:38])[CH:11]=2)=[CH:21][C:22]=1[O:34][CH3:35])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
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 4

HCID 8028TetrahydrofuranHCID 24414Barium SulfateHCID 537669791,5-Bis-(4-benzyloxy-3-methoxy-phenyl)-penta-1,4-dien-3-oneHCID 131709961Jones' reagent

生成物 1

HCID 187986361,5-Bis-(4-benzyloxy-3-methoxy-phenyl)-pentan-3-one

試薬・触媒・溶媒 3

HCID 23938
Palladium
触媒
HCID 180Acetone溶媒
HCID 3776Isopropanol溶媒

実験手順

Hydrogenation of 21.5 g (42.6 mmol) of 1,5-bis-(4-benzyloxy-3-methoxy-phenyl)-penta-1,4-dien-3-one prepared in Example D was effected as described in General Method 3 using 1.0 g 5% Pd over BaSO4 and 600 mL of THF under hydrogen atmosphere. The product contained both ketone and alcohol. Therefore, the mixture was dissolved in acetone (approximately 500 mL), treated with 20 mL of 8.0N Jones reagent, and stirred overnight at room temperature. Isopropanol was added, and the mixture was filtered through Celite. The filtrate was concentrated, and the residue was triturated with 1:1 hexane:EtOAc to give the title compound. 1H NMR (DMSO-d6) δ 2.71 (m, 8 H), 3.74 (s, 6 H), 5.02 (s, 4 H), 6.66 (m, 2 H), 6.82 (br s, 2 H), 6.87 (m, 2 H), 7.29-7.43 (m, 10 H).

後処理

  1. filtrationthe mixture was filtered through Celite
  2. concentrationThe filtrate was concentrated
  3. customthe residue was triturated with 1:1 hexane

出典と根拠

ORDレコード
ord-e58642045dff432ea8bd34052b6fb122
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05834506

反応ノート

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