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3-(1-Tritylimidazol-4-YL) propionaldehyde → 1-(5-fluorobenzo[b]thiophen-2-yl)-3-(1-triphenylmethyl-1H-imidazol-4-yl)-propan-1-ol

HRID 2229261
ノート
印刷プレビュー

反応式

HRID 2229261 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:5]2[S:6][CH:7]=[CH:8][C:4]=2[CH:3]=1.[Li]CCCC.[C:16]1([C:22]([C:38]2[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=2)([C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)[N:23]2[CH:27]=[C:26]([CH2:28][CH2:29][CH:30]=[O:31])[N:25]=[CH:24]2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1COCC1.[Cl-].[NH4+]>[F:1][C:2]1[CH:10]=[CH:9][C:5]2[S:6][C:7]([CH:30]([OH:31])[CH2:29][CH2:28][C:26]3[N:25]=[CH:24][N:23]([C:22]([C:38]4[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=4)([C:32]4[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=4)[C:16]4[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH:27]=3)=[CH:8][C:4]=2[CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 114514283-(1-Tritylimidazol-4-YL) propionaldehydeHCID 118159505-Fluoro-1-benzothiopheneHCID 178418339Butyllithium

生成物 1

HCID 184669791-(5-fluorobenzo[b]thiophen-2-yl)-3-(1-triphenylmethyl-1H-imidazol-4-yl)-propan-1-ol収率 62.2%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回
HCID 25517
Ammonium Chloride
溶媒

反応条件

温度
-40 °C

実験手順

To a solution of 5-fluorobenzo[b]thiophene (1.22 g) in THF (22 ml) was added n-BuLi (1.6 M solution in hexane, 5.0 ml) at −78° C., and the mixture was stirred for 1 hour. To this mixture was added a solution of 3-(1-triphenylmethyl-1H-imidazole-4-yl)propanal (2.93 g) in THF (10 ml), and the mixture was allowed to warm to −40° C. over 1 hour. The mixture was diluted with 10% aqueous ammonium chloride, warmed to room temperature, and extracted with ethyl acetate. The extract was washed with brine, dried over MgSO4, and concentrated. The residue was chromatographed on silica gel using hexane-ethyl acetate (1:1) as an eluent to give the titled compound as colorless crystals (2.58 g).

後処理

  1. temperaturewarmed to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-643722bb0a9f41fdb56f44091c46bd8b
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06420375B1

反応ノート

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