Triethylamine → HCID 70664099、化合物

HRID 1963082ノート

反応式

HRID 1963082 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[N:10][N:9]2[C:12]([C:30]([N:32]3[CH2:37][CH2:36][N:35]([C:38]([O:40][C:41]([CH3:44])([CH3:43])[CH3:42])=[O:39])[CH2:34][CH2:33]3)=[O:31])=[C:13]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:23]=3[CH3:29])[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)=[C:8]2[C:7]=1Cl)=[O:5])[CH3:2].C(N(CC)CC)C>C(O)C.C1COCC1.[Pd]>[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[N:10][N:9]2[C:12]([C:30]([N:32]3[CH2:33][CH2:34][N:35]([C:38]([O:40][C:41]([CH3:42])([CH3:44])[CH3:43])=[O:39])[CH2:36][CH2:37]3)=[O:31])=[C:13]([CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[C:24]([F:28])[C:23]=3[CH3:29])[C:14]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=3)=[C:8]2[CH:7]=1)=[O:5])[CH3:2]

参加物

5

反応物 2

HCID 8471TriethylamineHCID 67774159HCID 67774159、化合物

生成物 1

HCID 70664099HCID 70664099、化合物収率 93.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21873804Tetrahydrofuran ethanol溶媒

実験手順

The compound of step 9 (1.880 g, 2.96 mmol) in 29.6 ml of ethanol/THF (1:1) was hydrogenated under a hydrogen pressure of 2 bar for 3.5 h at room temperature in the presence of 0.315 g of 10% palladium on charcoal and triethylamine (0.62 ml, 4.44 mmol). The catalyst was filtered off and the filtrate was washed with brine (50 ml), dried with magnesium sulfate, filtered and concentrated to dryness under reduced pressure. 1.67 g of the title compound were obtained as a yellow solid.

後処理

  1. customfor 3.5 h
  2. customat room temperature
  3. filtrationThe catalyst was filtered off
  4. washthe filtrate was washed with brine (50 ml)
  5. dry with materialdried with magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-2e6aa282f1484d2190b1457e30038164
出典データセット
uspto-grants-2013_04
特許番号
US08415336B2

反応ノート

読み込み中…