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1,2-Dimethoxyethane → HCID 86633103、化合物

HRID 1012207
ノート
印刷プレビュー

反応式

HRID 1012207 の反応式
[F:1][C:2]([F:32])([F:31])[C:3]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:4]=1[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH:13]=[C:14]2[S:18][C:17](=[S:19])[NH:16][C:15]2=[O:20])=[CH:9][C:8]=1[O:21][CH3:22].COCCOC.[BH3-]C#N.[Na+].C([O-])(O)=O.[Na+]>CCOC(C)=O.C(O)(=O)C>[F:32][C:2]([F:1])([F:31])[C:3]1[CH:26]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:24]=[CH:23][C:4]=1[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]2[S:18][C:17](=[S:19])[NH:16][C:15]2=[O:20])=[CH:9][C:8]=1[O:21][CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 80711,2-DimethoxyethaneHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 72994854HCID 72994854、化合物

生成物 1

HCID 86633103HCID 86633103、化合物収率 368%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a N2-purged flask was added ′5-[1-[4-(2,4-bis-trifluoromethyl-benzyloxy)-3-methoxy-phenyl]-methylidene]-2-thioxo-thiazolidin-4-one (42 mg, 85 μmol) and DME (4 mL). To the solution was added NaBH3CN (20 mg, 255 μmol) followed by acetic acid (2 mL). The reaction was stirred at rt for 2 h. The reaction solution was then diluted with EtOAc (100 mL), neutralized by successive washings of sat NaHCO3 (100 mL×3), washed with sat. NaCl (100 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. The crude material was chromatographed (SiO2, DCM/MeOH 100:0 to 98:2) to provide intermediate compound (155 mg, 50% yield). 1H NMR (CDCl3) δ 9.29 (1H, br s), 7.99 (1H, d, J=8.1 Hz), 7.94 (1H, s), 7.83 (1H, d, J=8.1 Hz), 6.72-6.81 (3H, m), 5.38 (2H, s), 4.60 (1H, dd, J1=3.9 Hz, J2=9.8 Hz), 3.92 (3H, s), 3.48 (1H, dd, J=3.9 Hz, J2=14.2 Hz), 3.14 (1H, m); MS (ESI) 496 (MH+).

後処理

  1. customTo a N2-purged flask
  2. washwashed with sat. NaCl (100 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude material was chromatographed (SiO2, DCM/MeOH 100:0 to 98:2)

出典と根拠

ORDレコード
ord-4996c4ff91a74336a8a7700efd8f84dd
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977489B2

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