Hydrochloric Acid → HCID 86701773, 화합물

HRID 2174129노트

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HRID 2174129 반응식
[C:1]([C:3]([C:9]1[C:17]([O:18][CH3:19])=[CH:16][C:15]([CH3:20])=[C:14]2[C:10]=1[CH:11]=[CH:12][N:13]2[C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])([CH3:8])[C:4]([O:6]C)=[O:5])#[N:2].[OH-].[K+].Cl>CCO.O.C(OCC)(=O)C>[C:24]([O:23][C:21]([N:13]1[C:14]2[C:10](=[C:9]([C:3]([C:1]#[N:2])([CH3:8])[C:4]([OH:6])=[O:5])[C:17]([O:18][CH3:19])=[CH:16][C:15]=2[CH3:20])[CH:11]=[CH:12]1)=[O:22])([CH3:27])([CH3:25])[CH3:26]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 86701772HCID 86701772, 화합물

생성물 1

HCID 86701773HCID 86701773, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
0 °C

실험 절차

(±)-tert-Butyl 4-(2-cyano-1-methoxy-1-oxopropan-2-yl)-5-methoxy-7-methyl-1H-indole-1-carboxylate (Example 155-D) (0.35 g, 0.940 mmol) was dissolved in EtOH (4.70 ml), cooled to 0° C. and added 10% KOH (2.64 ml, 4.70 mmol) and stirred for 1 hour. At this point, the reaction was placed in an ice bath and quenched with 1 N HCl (4.70 ml, 4.70 mmol). The reaction was diluted with water and ethyl acetate. The layers were separated and the ethyl acetate layer was removed, dried over Na2SO4 and concentrated to obtain the title compound which was used directly in the next reaction without purification. MS (ESI+) m/z 359.4 (M+H).

후처리

  1. customAt this point, the reaction was placed in an ice bath
  2. customThe layers were separated
  3. customthe ethyl acetate layer was removed
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-31524c7067bb4a509061eecafb7bb3dc
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056874B2

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