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Ethyl Acetate → HCID 68313002、化合物

HRID 1530440
ノート
印刷プレビュー

反応式

HRID 1530440 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].C([O:14][C:15](=O)[C:16]([O:28][C:29]1[CH:51]=[CH:50][C:32]2[C:33]3[N:37]([CH2:38][CH2:39][O:40][C:31]=2[CH:30]=1)[CH:36]=[C:35]([C:41]1[N:42]([CH:47]([CH3:49])[CH3:48])[N:43]=[C:44]([CH3:46])[N:45]=1)[N:34]=3)([CH3:27])[CH2:17][CH2:18][O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)C1C=CC=CC=1.CCOC(C)=O.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1COCC1>[CH2:20]([O:19][CH2:18][CH2:17][C:16]([O:28][C:29]1[CH:51]=[CH:50][C:32]2[C:33]3[N:37]([CH2:38][CH2:39][O:40][C:31]=2[CH:30]=1)[CH:36]=[C:35]([C:41]1[N:42]([CH:47]([CH3:49])[CH3:48])[N:43]=[C:44]([CH3:46])[N:45]=1)[N:34]=3)([CH3:27])[CH2:15][OH:14])[C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8857Ethyl AcetateHCID 9357Potassium Sodium TartrateHCID 21226445Aluminium lithium hydrideHCID 68312931HCID 68312931、化合物

生成物 1

HCID 68313002HCID 68313002、化合物収率 98%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

To a suspension of LiAlH4 (4.4 mg, 0.116 mmol) in THF (1 mL) was added a solution of 4-benzyloxy-2-[2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]-2-methylbutyric acid benzyl ester (36 mg, 0.058 mmol) in THF (2 mL) and stirring at RT was continued for 2.5 h. To the reaction mixture was added EtOAc (0.5 mL) and stirring was continued for 10 min. An aqueous solution of Rochelle's salt was then added and the aqueous phase was extracted with EtOAc (×2). 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 3-12% MeOH in DCM) affording 4-Benzyloxy-2-[2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-8-yloxy]-2-methylbutan-1-ol (29 mg, 98%). 1H NMR (CDCl3, 400 MHz): δ 8.41 (1H, d, J=8.83 Hz), 7.60 (1H, s), 7.39-7.27 (5H, m), 6.81 (1H, dd, J=8.83, 2.41 Hz), 6.69 (1H, d, J=2.37 Hz), 5.98-5.85 (1H, m), 4.60-4.50 (2H, m), 4.49-4.35 (4H, m), 3.83-3.69 (2H, m), 3.65-3.55 (2H, m), 3.24 (1H, s), 2.42 (3H, s), 2.20-2.12 (1H, m), 2.07-1.97 (1H, m), 1.57 (6H, d, J=6.75 Hz), 1.31 (3H, s)

後処理

  1. stirringstirring
  2. waitwas continued for 10 min
  3. extractionthe aqueous phase was extracted with EtOAc (×2)
  4. washThe combined organic phases were washed with water
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated in vacuo
  7. customThe resulting residue was purified by column chromatography (Si-PCC, gradient 3-12% MeOH in DCM)

出典と根拠

ORDレコード
ord-f06da8b3d6b645c381adec5b1136d71d
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

読み込み中…

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