4-[7-(Benzyl)-1-(ethoxycarbonylmethyl)-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester → 4-[1-(Ethoxycarbonylmethyl)-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

HRID 1792019ノート

反応式

HRID 1792019 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[N:22](CC3C=CC=CC=3)[C:21]3[C:20](=[O:30])[N:19]([CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[C:18](=[O:37])[N:17]([CH3:38])[C:16]=3[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)(=O)C.[OH-].[Pd+2].[OH-]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[NH:22][C:21]3[C:20](=[O:30])[N:19]([CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[C:18](=[O:37])[N:17]([CH3:38])[C:16]=3[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:3])([CH3:4])[CH3:2]

参加物

4

反応物 1

HCID 235369644-[7-(Benzyl)-1-(ethoxycarbonylmethyl)-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

生成物 1

HCID 235369654-[1-(Ethoxycarbonylmethyl)-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 176Acetic Acid溶媒

実験手順

4-[7-Benzyl-1-(ethoxycarbonylmethyl)-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl]piperazine-1-carboxylic acid tert-butyl ester was dissolved in acetic acid, and palladium hydroxide (ca. 10 mg) was added thereto. The reaction mixture was stirred at room temperature under hydrogen atmosphere overnight, filtered, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, and washed with saturated aqueous solution of sodium bicarbonate. The organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure to give 111 mg of the title compound.

後処理

  1. filtrationfiltered
  2. concentrationthe filtrate was concentrated
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with saturated aqueous solution of sodium bicarbonate
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-4374c8aae1004adb81c7f8b9ff4f53f8
出典データセット
uspto-grants-2006_07
特許番号
US07074798B2

反応ノート

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