Potassium Carbonate → N-Cyclohexyl-N-(2,2-dimethoxyethyl)-3-(3-(oxazol-5-yl)phenethoxy)propanamide

HRID 909908노트

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HRID 909908 반응식
[CH:1]1([N:7]([CH2:23][CH:24]([O:27][CH3:28])[O:25][CH3:26])[C:8](=[O:22])[CH2:9][CH2:10][O:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([CH:20]=[O:21])[CH:15]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1(C)C(S([CH2:38][N+:39]#[C-:40])(=O)=O)=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH:1]1([N:7]([CH2:23][CH:24]([O:27][CH3:28])[O:25][CH3:26])[C:8](=[O:22])[CH2:9][CH2:10][O:11][CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([C:20]3[O:21][CH:40]=[N:39][CH:38]=3)[CH:15]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 53627694Toluenesulfonylmethyl isocyanideHCID 59290390N-Cyclohexyl-N-(2,2-dimethoxyethyl)-3-(3-formylphenethoxy)propanamide

생성물 1

HCID 59290488N-Cyclohexyl-N-(2,2-dimethoxyethyl)-3-(3-(oxazol-5-yl)phenethoxy)propanamide

시약·촉매·용매 1

HCID 887Methanol용매

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온도
80 °C

실험 절차

To N-cyclohexyl-N-(2,2-dimethoxyethyl)-3-(3-formylphenethoxy)propanamide [Example 10, Step ii)] (600 mg) in a 10 ml microwave vial was added toluenesulfonylmethyl isocyanide (329 mg), potassium carbonate (233 mg) and methanol (2 mL). The vial was sealed and heated at 80° C. for 40 min within a microwave before cooling to room temperature. The solvents were evaporated under vacuum followed by the addition of water, which was extracted once with ethyl acetate. The organic phase was washed once with water, dried over sodium sulphate, filtered and the solvent removed to afford desired material, which was carried onto the next step directly. MS [M+H-MeOH]+=399 (MultiMode+)

후처리

  1. customThe vial was sealed
  2. temperaturebefore cooling to room temperature
  3. customThe solvents were evaporated under vacuum
  4. additionfollowed by the addition of water, which
  5. extractionwas extracted once with ethyl acetate
  6. washThe organic phase was washed once with water
  7. dry with materialdried over sodium sulphate
  8. filtrationfiltered
  9. customthe solvent removed
  10. customto afford desired material, which

출처 및 근거

ORD 기록
ord-fa6f00f8c2134d03a0deeae3bea3d519
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08017602B2

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