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

HRID 1107185
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HRID 1107185 반응식
[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
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

(±)-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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-b5941e8ee76e489b8961746522104807
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057369

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