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3-{1-[6-(3-bromo-7,8-dihydro-5H-1,6-naphthyridin-6-carbonyl)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one → 3-{1-[6-(7,8-dihydro-5H-1,6-naphthyridin-6-carbonyl)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

HRID 74644
ノート
印刷プレビュー

反応式

HRID 74644 の反応式
Br[C:2]1[CH:3]=[N:4][C:5]2[CH2:6][CH2:7][N:8]([C:12]([C:14]3[N:19]=[CH:18][N:17]=[C:16]([N:20]4[CH2:25][CH2:24][CH:23]([N:26]5[CH2:32][CH2:31][C:30]6[CH:33]=[C:34]([O:37][CH3:38])[CH:35]=[CH:36][C:29]=6[NH:28][C:27]5=[O:39])[CH2:22][CH2:21]4)[CH:15]=3)=[O:13])[CH2:9][C:10]=2[CH:11]=1.[H][H]>[Pd].CO>[N:4]1[C:5]2[CH2:6][CH2:7][N:8]([C:12]([C:14]3[N:19]=[CH:18][N:17]=[C:16]([N:20]4[CH2:25][CH2:24][CH:23]([N:26]5[CH2:32][CH2:31][C:30]6[CH:33]=[C:34]([O:37][CH3:38])[CH:35]=[CH:36][C:29]=6[NH:28][C:27]5=[O:39])[CH2:22][CH2:21]4)[CH:15]=3)=[O:13])[CH2:9][C:10]=2[CH:11]=[CH:2][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 583866353-{1-[6-(3-bromo-7,8-dihydro-5H-1,6-naphthyridin-6-carbonyl)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 426134533-{1-[6-(7,8-dihydro-5H-1,6-naphthyridin-6-carbonyl)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒
HCID 887
Methanol
溶媒

実験手順

Under a hydrogen atmosphere 77 mg (0.12 mmol) 3-{1-[6-(3-bromo-7,8-dihydro-5H-1,6-naphthyridin-6-carbonyl)-pyrimidin-4-yl]-piperidin-4-yl}-7-methoxy-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 40 mg palladium on charcoal (10%) were hydrogenated in 10 mL methanol at 50° C. under 50 psi hydrogen pressure. Then the catalyst was removed by suction filtering and the filtrate was evaporated down i. vac. The residue was purified by preparative HPLC. The product fractions were combined and lyophilised.

後処理

  1. customThen the catalyst was removed by suction
  2. filtrationfiltering
  3. customthe filtrate was evaporated down i
  4. customThe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-a7ee3a2fda2a4339966f01710926ccbb
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829006B2

反応ノート

読み込み中…

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