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HCID 10209327, 화합물 → Acat-IN-2

HRID 2289675
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HRID 2289675 반응식
[CH:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[C:6]([CH:13]([CH3:15])[CH3:14])[C:5]=1[O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]1[C:26]([CH:27]([CH3:29])[CH3:28])=[CH:25][C:24]([CH:30]([CH3:32])[CH3:31])=[CH:23][C:22]=1[CH:33]([CH3:35])[CH3:34])([CH3:3])[CH3:2].[H][H]>[Ni].O1CCCC1.C(OCC)(=O)C>[NH2:10][C:8]1[CH:9]=[C:4]([CH:1]([CH3:3])[CH3:2])[C:5]([O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]2[C:22]([CH:33]([CH3:34])[CH3:35])=[CH:23][C:24]([CH:30]([CH3:31])[CH3:32])=[CH:25][C:26]=2[CH:27]([CH3:29])[CH3:28])=[C:6]([CH:13]([CH3:15])[CH3:14])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 10209327HCID 10209327, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 10142595Acat-IN-2수율 89.5%

시약·촉매·용매 3

HCID 935Nickel촉매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

22.0 g of [(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 2,6-diisopropyl-4-nitro-phenyl ester and 6 g of Raney nickel were mixed in 110 mL tetrahydrofuran under 50 psi of hydrogen. After 21 hours, the reaction was filtered and concentrated to give an orange oil which was dissolved in ethyl acetate, filtered through a pad of silica, and concentrated to give an oily solid. Recrystallization from 53 diethyl ether/hexanes gave 18.60 g (89%) of the title compound as a cream colored solid; mp 153-155° C.

후처리

  1. filtrationthe reaction was filtered
  2. concentrationconcentrated
  3. customto give an orange oil which
  4. filtrationfiltered through a pad of silica
  5. concentrationconcentrated
  6. customto give an oily solid
  7. customRecrystallization from 53 diethyl ether/hexanes

출처 및 근거

ORD 기록
ord-1007f16de5304b9b87ded69af7cb09de
출처 데이터셋
uspto-grants-2000_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06093744

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