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Water → 9-(1-bromoethyl)-8-fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene

HRID 1530731
ノート
印刷プレビュー

反応式

HRID 1530731 の反応式
P(Br)(Br)[Br:2].[F:5][C:6]1[C:28]([CH:29](O)[CH3:30])=[CH:27][C:9]2[C:10]3[N:14]([CH2:15][CH2:16][O:17][C:8]=2[CH:7]=1)[CH:13]=[C:12]([C:18]1[N:19]([CH:24]([CH3:26])[CH3:25])[N:20]=[C:21]([CH3:23])[N:22]=1)[N:11]=3.O.C([O-])(O)=O.[Na+]>C(Cl)Cl>[Br:2][CH:29]([C:28]1[C:6]([F:5])=[CH:7][C:8]2[O:17][CH2:16][CH2:15][N:14]3[C:10](=[N:11][C:12]([C:18]4[N:19]([CH:24]([CH3:26])[CH3:25])[N:20]=[C:21]([CH3:23])[N:22]=4)=[CH:13]3)[C:9]=2[CH:27]=1)[CH3:30]
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 962WaterHCID 24614Phosphorus tribromideHCID 516892Sodium BicarbonateHCID 683128551-[8-Fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-9-yl]ethanol

生成物 1

HCID 683131309-(1-bromoethyl)-8-fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene収率 88%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Phosphorus tribromide (0.53 mL of a 1.0 M solution in DCM) was added to a solution of 1-[8-fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulen-9-yl]ethanol (98 mg, 0.26 mmol) in DCM (1 mL) at 0° C. The mixture was warmed to RT and stirred for 20 h. Water (2 mL) and sat. NaHCO3 (2 mL) were added and the mixture was extracted with DCM. The combined organics were washed (brine), dried (Na2SO4) and concentrated in vacuo to give the title compound (100 mg, 0.23 mmol, 88%) as a pale yellow solid. The product was taken on without further purification. 1H NMR (CDCl3, 300 MHz): δ 8.72 (1H, d, J=8.7 Hz), 7.60 (1H, s), 6.75 (1H, d, J=11.0 Hz), 5.82 (1H, sept., J=6.6 Hz), 5.45 (1H, q, J=7.0 Hz), 4.52-4.49 (2H, m), 4.44-4.41 (2H, m), 2.42 (3H, s), 2.11 (3H, d, J=7.0 Hz), 1.60 (6H, d, J=6.6 Hz)

後処理

  1. extractionthe mixture was extracted with DCM
  2. washThe combined organics were washed (brine)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2cbb9fc1763d4dcd8e4761afda20e42e
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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