Water → 5-[1-(cyclopropylmethyl)-4-(trifluoromethyl)-1H-benzotriazol-5-yl]-6-fluoropyridine-2-carbaldehyde

HRID 2281041ノート

反応式

HRID 2281041 の反応式
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([C:18]4[CH:19]=[CH:20][C:21]([CH:25]([OH:28])CO)=[N:22][C:23]=4[F:24])=[C:13]([C:14]([F:17])([F:16])[F:15])[C:8]=3[N:7]=[N:6]2)[CH2:3][CH2:2]1.O.I([O-])(=O)(=O)=O.[Na+]>C(#N)C>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([C:18]4[CH:19]=[CH:20][C:21]([CH:25]=[O:28])=[N:22][C:23]=4[F:24])=[C:13]([C:14]([F:16])([F:15])[F:17])[C:8]=3[N:7]=[N:6]2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 962WaterHCID 23667635Sodium periodateHCID 709782561-{5-[1-(cyclopropylmethyl)-4-(trifluoromethyl)-1H-benzotriazol-5-yl]-6-fluoropyridin-2-yl}ethane-1,2-diol

生成物 1

HCID 867119795-[1-(cyclopropylmethyl)-4-(trifluoromethyl)-1H-benzotriazol-5-yl]-6-fluoropyridine-2-carbaldehyde

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1-{5-[1-(Cyclopropylmethyl)-4-(trifluoromethyl)-1H-benzotriazol-5-yl]-6-fluoropyridin-2-yl}ethane-1,2-diol (32 mg, 0.081 mmol) was dissolved in acetonitrile (1 ml) and deionized water (0.5 mL), cooled to 0° C. and treated with sodium periodate (19 mg, 0.089 mmol, 1.1 equiv). The ice bath was removed and the mixture was warmed to ambient temperature and stirred for 1 hour, which was diluted with ethyl acetate (30 mL) and washed with sodium bicarbonate (2×15 mL, aqueous saturated). The combined organic extracts were dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

後処理

  1. customThe ice bath was removed
  2. additionwhich was diluted with ethyl acetate (30 mL)
  3. washwashed with sodium bicarbonate (2×15 mL, aqueous saturated)
  4. dry with materialThe combined organic extracts were dried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f6da89be33f3442d9adb3107cc63f44d
出典データセット
uspto-grants-2015_09
特許番号
US09139576B2

反応ノート

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