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

HRID 1846550
ノート
印刷プレビュー

反応式

HRID 1846550 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]([CH:37]4[CH2:39][CH2:38]4)[NH:34][C:33]=3[CH:40]=2)[CH:23]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[CH:37]1([C:35]2[NH:34][C:33]3[CH:40]=[C:29]([O:28][C:24]4[N:25]=[CH:26][N:27]=[C:22]([N:17]5[CH2:18][CH2:19][CH:14]([N:10]6[CH2:9][CH2:8][C:7]7[CH:20]=[C:3]([O:2][CH3:1])[CH:4]=[CH:5][C:6]=7[NH:12][C:11]6=[O:13])[CH2:15][CH2:16]5)[CH:23]=4)[CH:30]=[C:31]([CH3:41])[C:32]=3[N:36]=2)[CH2:38][CH2:39]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 3

HCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 866639156-(6-chloropyrimidin-4-yloxy)-2-cyclopropyl-4-methyl-1H-benzo[d]imidazole

生成物 1

HCID 462447623-{1-[6-(2-cyclopropyl-4-methyl-1H-benzo[d]imidazol-6-yloxy)pyrimidin-4-yl]piperidin-4-yl}-7-methoxy-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

44 mg (0.16 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 40 mg (0.13 mmol) 6-(6-chloropyrimidin-4-yloxy)-2-cyclopropyl-4-methyl-1H-benzo[d]imidazole and 0.06 mL (0.32 mmol) DIPEA in 2.0 mL DMF were stirred overnight at RT. The reaction mixture was purified by preparative HPLC-MS. The fractions containing the 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 the 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-5c9e204a76d0416aa947e9fefe1bbe7f
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952014B2

反応ノート

読み込み中…

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