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Ethyl Acetate → N-(((3S,4R,5S)-3-(2-fluorophenyl)-4-(hydroxymethyl)-5-(trifluoromethyl)tetrahydrofuran-3-yl)carbamothioyl)benzamide

HRID 2045879
ノート
印刷プレビュー

反応式

HRID 2045879 の反応式
C(O[C@@H]([C@H](OC(=O)C1C=CC=CC=1)C(O)=O)C(O)=O)(=O)C1C=CC=CC=1.[NH2:27][C@@:28]1([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][C:40]=2[F:45])[CH2:32][O:31][C@H:30]([C:33]([F:36])([F:35])[F:34])[C@H:29]1[CH2:37][OH:38].CCOC(C)=O.[OH-].[Na+].[C:54]([N:62]=[C:63]=[S:64])(=[O:61])[C:55]1[CH:60]=[CH:59][CH:58]=[CH:57][CH:56]=1>C(Cl)Cl>[F:45][C:40]1[CH:41]=[CH:42][CH:43]=[CH:44][C:39]=1[C@@:28]1([NH:27][C:63]([NH:62][C:54](=[O:61])[C:55]2[CH:56]=[CH:57][CH:58]=[CH:59][CH:60]=2)=[S:64])[C@H:29]([CH2:37][OH:38])[C@@H:30]([C:33]([F:36])([F:34])[F:35])[O:31][CH2:32]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 4

HCID 8857Ethyl Acetate2 回HCID 14798Sodium HydroxideHCID 68284Benzoyl isothiocyanateHCID 86668368((2S,3R,45)-4-Amino-4-(2-fluorophenyl)-2-(trifluoromethyl)tetrahydrofuran-3-yl)methanol (2S,3S)-2,3-bis(benzoyloxy)succinate

生成物 1

HCID 60169627N-(((3S,4R,5S)-3-(2-fluorophenyl)-4-(hydroxymethyl)-5-(trifluoromethyl)tetrahydrofuran-3-yl)carbamothioyl)benzamide
収率 106.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-3 °C

実験手順

To chiral salt ((2S,3R,4S)-4-Amino-4-(2-fluorophenyl)-2-(trifluoromethyl)tetrahydrofuran-3-yl)methanol (2S,3S)-2,3-bis(benzoyloxy)succinate (0.361 kg, 0.556 mol) was added EtOAc (1.08 L) and the suspension was cooled to −3° C. 1.0 N aq. NaOH (1.30 L) was added over 20 mins while maintaining T<5° C. After 5 mins, benzoyl isothiocyanate (80.0 mL, 594 mmol) was added over 8 mins while maintaining T<5° C. After 1 h, EtOAc (722 mL) was charged. The aq. layer was removed, and the organics were washed with sat. aq. NaHCO3 (361 mL) and sat. aq. NaCl (361 mL). The organics were filtered over celite (90 g) and rinsed with EtOAc (360 mL). The organics were concentrated under vacuum to afford a residue which was re-dissolved into CH2Cl2 (1.1 L) and concentrated to afford the title compound as yellow foam (261 g, 99% yield accounting for residual solvents) which was used in the following step. 1H NMR (500 MHz, DMSO) δ ppm 12.04 (s, 2H), 11.20 (s, 2H), 7.95 (d, J=7.4 Hz, 2H), 7.69-7.60 (m, 1H), 7.56-7.42 (m, 2H), 7.37-7.28 (m, 1H), 7.24-7.12 (m, 2H). 5.59 (t, J=4.5 Hz, 1H), 5.03 (d, J=9.7 Hz, 1H), 4.92 (d, J=9.7 Hz, 1H), 4.75-4.63 (m, 1H), 3.92-3.74 (m, 2H), 2.77-2.66 (m, 1H); 13C NMR (125 MHz, DMSO) δ ppm 179.98, 167.85, 159.75 (d, JCF=245.0 Hz), 133.44, 132.58, 129.88, 129.81, 129.04, 128.85, 126.31 (d, JCF=9.8 Hz), 124.36, 116.83 (d, JCF=23.4 Hz), 76.11 (q, JCF=31.0 Hz). 74.37 (d, JCF=6.1 Hz), 68.77 (d, JCF=3.4 Hz), 57.03, 52.23.

後処理

  1. temperaturewhile maintaining T<5° C
  2. temperaturewhile maintaining T<5° C
  3. waitAfter 1 h
  4. customThe aq. layer was removed
  5. washthe organics were washed with sat. aq. NaHCO3 (361 mL) and sat. aq. NaCl (361 mL)
  6. filtrationThe organics were filtered over celite (90 g)
  7. washrinsed with EtOAc (360 mL)
  8. concentrationThe organics were concentrated under vacuum
  9. customto afford a residue which
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-793a243772c74ee1b58f82f44cbb1dcd
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08592408B2

反応ノート

読み込み中…

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