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Oxalyl chloride → (+/-)-3-(4-Methoxyphenylsulfanyl)-2-methyl-7-phenylheptanoic acid hydroxyamide

HRID 1107185
ノート
印刷プレビュー

反応式

HRID 1107185 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9][CH:10]([CH2:16][CH2:17][CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:11]([CH3:15])[C:12](O)=[O:13])=[CH:5][CH:4]=1.C(Cl)(=O)C(Cl)=O.C[Si](C)(C)[O:34][NH2:35]>C(Cl)Cl>[OH:34][NH:35][C:12](=[O:13])[CH:11]([CH3:15])[CH:10]([S:9][C:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)[CH2:16][CH2:17][CH2:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=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

5

反応物 3

HCID 65578Oxalyl chlorideHCID 2734666O-(Trimethylsilyl)hydroxylamineHCID 18790075(+/-)-3-(4-Methoxyphenylsulfanyl)-2-methyl-7-phenylheptanoic acid

生成物 1

HCID 17915535(+/-)-3-(4-Methoxyphenylsulfanyl)-2-methyl-7-phenylheptanoic acid hydroxyamide収率 90.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

(±)-3-(4-Methoxyphenylsulfanyl)-2-methyl-7-phenylheptanoic acid (0.38 g, 1.1 mmol) is dissolved in CH2Cl2 (1 mL) and cooled to 0° C. A solution of oxalyl chloride in CH2Cl2 (0.7 mL, 1.4 mmol) is added dropwise, the bath removed and the reaction allowed to warm and stir at 23° C. for 3 hours. The reaction is then concentrated in vacuo and azeotroped with CHCl3. The resulting oil is dissolved in CH2Cl2 (3 mL), cooled to 0° C. and O-(trimethylsilyl)hydroxylamine (0.4 mL, 3.4 mmol) is added dropwise. The bath is removed and the reaction is allowed to warm to 20° C. The reaction is then partitioned between CH2Cl2 (20 mL) and 1 N HCl (10 mL). The organic layer is then separated and washed with water (10 mL), dried (MgSO4) and concentrated in vacuo to yield (±)-3-(4-methoxyphenylsulfanyl)-2-methyl-7-phenylheptanoic acid hydroxyamide (0.37 g, 90%) which is used without further purification: 1H NMR (300 MHz, CDCl3) δ 7.30-7.18 (m, 4H), 7.14-7.07 (m, 3H), 7.80-7.73 (m, 2H), 3.73 (s, 1.5H), 3.72 (s, 1.5H), 3.12-3.06 (m, 0.5H), 2.97-2.90 (m, 0.5H), 2.53 (m, 2H), 2.32-2.19 (m, 1H), 1.68-1.25 (m, 6H) 1.16 (d, J=7.0 Hz, 1.5H), 1.11 (d, J=7.0 Hz, 1.5H); MS (FAB) m/e 374 (M+H)+.

後処理

  1. customthe bath removed
  2. temperatureto warm
  3. concentrationThe reaction is then concentrated in vacuo
  4. customazeotroped with CHCl3
  5. dissolutionThe resulting oil is dissolved in CH2Cl2 (3 mL)
  6. temperaturecooled to 0° C.
  7. customThe bath is removed
  8. temperatureto warm to 20° C
  9. customThe reaction is then partitioned between CH2Cl2 (20 mL) and 1 N HCl (10 mL)
  10. customThe organic layer is then separated
  11. washwashed with water (10 mL)
  12. dry with materialdried (MgSO4)
  13. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b5941e8ee76e489b8961746522104807
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06057369

反応ノート

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