7-benzyl-8-methyl-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine → 8-methyl-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine

HRID 510237ノート

反応式

HRID 510237 の反応式
C([N:8]1[CH2:17][CH2:16][C:15]2[C:14]([C:18]3[N:22]([CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][O:24]4)[N:21]=[CH:20][CH:19]=3)=[N:13][CH:12]=[N:11][C:10]=2[CH:9]1[CH3:29])C1C=CC=CC=1.[H][H]>CCO.[Pd]>[CH3:29][CH:9]1[C:10]2[N:11]=[CH:12][N:13]=[C:14]([C:18]3[N:22]([CH:23]4[CH2:28][CH2:27][CH2:26][CH2:25][O:24]4)[N:21]=[CH:20][CH:19]=3)[C:15]=2[CH2:16][CH2:17][NH:8]1

参加物

5

反応物 2

HCID 904079497-benzyl-8-methyl-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidineHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 904082318-methyl-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidine収率 98.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 702Ethanol溶媒

実験手順

To the product of Example 112, step f (356 mg, 0.91 mmol) in EtOH (9 mL) was added a catalytic amount of 10% Pd/C Degussa type followed by a balloon of hydrogen gas. The mixture was stirred at room temperature overnight. The balloon was refilled with hydrogen gas and an additional spatula tip of 10% Pd/C was added. After an additional 24 h and the reaction was complete. The catalyst was removed by filtration and the liquid was concentrated in vacuo to afford the desired product (268 mg, 98%). MS (ESI) mass calcd. C16H21N5O, 299.2. m/z found 300.2 [M+H]+.

後処理

  1. waitAfter an additional 24 h
  2. customThe catalyst was removed by filtration
  3. concentrationthe liquid was concentrated in vacuo

出典と根拠

ORDレコード
ord-00fecfc48ee94fdd90499d0b6b30bd80
出典データセット
uspto-grants-2015_08
特許番号
US09096596B2

反応ノート

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