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Triethylamine → HCID 178453873、化合物

HRID 1664861
ノート
印刷プレビュー

反応式

HRID 1664861 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C@H:9]1[CH2:15][NH:14][C:13](=S)[C@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]1.[Cl-].[F:26][C:27]([F:34])([F:33])[CH2:28][CH:29]([OH:32])[CH2:30][NH3+:31].C(N(CC)CC)C>C(O)C.[Hg](Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([F:8])[C:3]=1[C@H:9]1[CH2:15][NH:14]/[C:13](=[N:31]\[CH2:30][CH:29]([OH:32])[CH2:28][C:27]([F:34])([F:33])[F:26])/[C@H:12]([NH:17][C:18](=[O:24])[O:19][C:20]([CH3:23])([CH3:22])[CH3:21])[CH2:11][CH2:10]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 3

HCID 8471TriethylamineHCID 59722652HCID 59722652、化合物HCID 866167544,4,4-Trifluoro-2-hydroxybutan-1-aminium chloride

生成物 1

HCID 178453873HCID 178453873、化合物

試薬・触媒・溶媒 2

HCID 24085Mercuric Chloride触媒HCID 702Ethanol溶媒

実験手順

Mercury(II) chloride (538 mg, 1.98 mmol) was added to a solution of tert-butyl [(3R,6S)-6-(2,6-difluorophenyl)-2-thioxoazepan-3-yl]carbamate (353 mg, 0.99 mmol), 4,4,4-trifluoro-2-hydroxybutan-1-aminium chloride (498 mg, 2.77 mmol), and triethylamine (0.61 mL, 4.36 mmol) in ethanol (10 mL) at 55° C. After 2 h, the reaction was allowed to cool to ambient temperature. The mixture was filtered and concentrated. Saturated aqueous sodium bicarbonate was added and the mixture was extracted with dichloromethane (2×). The combined organic extracts were dried over magnesium sulfate, filtered, and concentrated to give the title compound. MS 466.2 (M+1).

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. additionSaturated aqueous sodium bicarbonate was added
  4. extractionthe mixture was extracted with dichloromethane (2×)
  5. dry with materialThe combined organic extracts were dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-6611fbef944648fe97e802705b3286ad
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039460B2

反応ノート

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