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Sodium hydride → HCID 68312871、化合物

HRID 1530694
ノート
印刷プレビュー

反応式

HRID 1530694 の反応式
C(OC(N1CCC(C([O:20][C:21]2[CH:43]=[CH:42][C:24]3[C:25]4[N:29]([CH2:30][CH2:31][O:32][C:23]=3[CH:22]=2)[CH:28]=[C:27]([C:33]2[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=2)[N:26]=4)CC)CC1)=O)C1C=CC=CC=1.[H-].[Na+].[CH2:46]([O:48][C:49](=[O:61])[C:50](Br)([CH2:56][CH:57]1[CH2:59][CH2:58]1)[C:51]([O:53][CH2:54][CH3:55])=[O:52])[CH3:47]>CN(C=O)C>[CH2:46]([O:48][C:49](=[O:61])[C:50]([CH2:56][CH:57]1[CH2:59][CH2:58]1)([O:20][C:21]1[CH:43]=[CH:42][C:24]2[C:25]3[N:29]([CH2:30][CH2:31][O:32][C:23]=2[CH:22]=1)[CH:28]=[C:27]([C:33]1[N:34]([CH:39]([CH3:41])[CH3:40])[N:35]=[C:36]([CH3:38])[N:37]=1)[N:26]=3)[C:51]([O:53][CH2:54][CH3:55])=[O:52])[CH3:47]
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 24758Sodium hydride2 回HCID 68312705HCID 68312705、化合物2 回HCID 68312962HCID 68312962、化合物2 回

生成物 1

HCID 68312871HCID 68312871、化合物収率 187.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a suspension of 2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol from Example 4 (100 mg, 0.307 mmol) in DMF (2 mL) was added sodium hydride (12.3 mg, 60% in oil, 0.307 mmol). The mixture was stirred at RT for 15 min, then 2-bromo-2-cyclopropylmethylmalonic acid diethyl ester (135 mg, 0.46 mmol) was added. The reaction mixture was stirred at RT for 1 h, and then at 70° C. for 6 h. The reaction was repeated with 2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-ol from Example 4 (400 mg, 1.23 mmol), DMF (8 mL), sodium hydride (49.2 mg, 1.23 mmol) and 2-bromo-2-cyclopropylmethylmalonic acid diethyl ester (540 mg, 1.84 mmol). The cooled reaction mixtures were combined and partitioned between water and EtOAc. The aqueous phase was extracted with EtOAc. The combined organic phases were washed with water, followed by brine, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si-PCC, gradient 2-10% MeOH in DCM) affording the title compound (0.309 g, 37%). LCMS (Method B): RT 3.77 min [M+H]+ 538.

後処理

  1. stirringThe reaction mixture was stirred at RT for 1 h
  2. waitat 70° C. for 6 h
  3. customThe cooled reaction mixtures
  4. custompartitioned between water and EtOAc
  5. extractionThe aqueous phase was extracted with EtOAc
  6. washThe combined organic phases were washed with water
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated in vacuo
  9. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 2-10% MeOH in DCM)

出典と根拠

ORDレコード
ord-603fd0d9df5c46068003fd529a84b6c3
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート