Diisopropylethylamine → 7-methoxy-3-{1-[6-(2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-yloxy)pyrimidin-4-yl]piperidin-4-yl}-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-one

HRID 1846546ノート

反応式

HRID 1846546 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1.Cl[C:22]1[N:27]=[CH:26][N:25]=[C:24]([O:28][C:29]2[CH:30]=[C:31]([CH3:41])[C:32]3[N:36]=[C:35]([CH2:37][O:38][CH3:39])[NH:34][C:33]=3[CH:40]=2)[CH:23]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][N:17]([C:22]4[CH:23]=[C:24]([O:28][C:29]5[CH:30]=[C:31]([CH3:41])[C:32]6[N:36]=[C:35]([CH2:37][O:38][CH3:39])[NH:34][C:33]=6[CH:40]=5)[N:25]=[CH:26][N:27]=4)[CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 866639136-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole

生成物 1

HCID 462447587-methoxy-3-{1-[6-(2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazol-6-yloxy)pyrimidin-4-yl]piperidin-4-yl}-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

52 mg (0.19 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 50 mg (0.16 mmol) 6-(6-chloropyrimidin-4-yloxy)-2-(methoxymethyl)-4-methyl-1H-benzo[d]imidazole and 0.07 mL (0.40 mmol) DIPEA in 2.0 mL DMF were stirred at RT over the weekend. The reaction mixture was purified by preparative HPLC-MS. The fractions containing product were partially evaporated down i.vac. and neutralised with 4M sodium hydroxide solution. The precipitate formed was suction filtered, washed and dried.

後処理

  1. customThe reaction mixture was purified by preparative HPLC-MS
  2. additionThe fractions containing product
  3. customwere partially evaporated down i.vac
  4. customThe precipitate formed
  5. filtrationfiltered
  6. washwashed
  7. customdried

出典と根拠

ORDレコード
ord-37a638ea44d546bcbd21aab6574c4caa
出典データセット
uspto-grants-2015_02
特許番号
US08952014B2

反応ノート

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