Tert-butyl 3-aminoazetidine-1-carboxylate → HCID 58777638, 화합물

HRID 1371775노트

반응식

HRID 1371775 반응식
[NH2:1][C:2]1[C:7]([C:8]([C:10]2[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=2[F:19])=[O:9])=[CH:6][N:5]=[C:4](Cl)[N:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH2:32])[CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(Cl)Cl.C(O)C>[C:21]([O:25][C:26]([N:28]1[CH2:31][CH:30]([NH:32][C:4]2[N:3]=[C:2]([NH2:1])[C:7]([C:8](=[O:9])[C:10]3[C:15]([O:16][CH3:17])=[CH:14][CH:13]=[C:12]([F:18])[C:11]=3[F:19])=[CH:6][N:5]=2)[CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

참가 물질

5

반응물 2

HCID 1516507Tert-butyl 3-aminoazetidine-1-carboxylateHCID 21070550HCID 21070550, 화합물

생성물 1

HCID 58777638HCID 58777638, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

반응 조건

온도
80 °C

실험 절차

To a stirred suspension of chloropyrimidine (700 mg, 2.34 mmol, Example 289) in methylene chloride (30 mL), amine (525 mg, 5.64 mmol, Example 318) in ethanol (30 mL) was added and the mixture heated at 80° C. for 4.5 hours. The solvent was removed and the residue was dissolved in ethyl acetate and the mixture was washed successively with 0.5N hydrochloric acid and water. The organic layer was dried with sodium sulfate and concentrated to give a white solid. 1.0 g, 98%. MS (ES) MH+=436.

후처리

  1. additionwas added
  2. customThe solvent was removed
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washthe mixture was washed successively with 0.5N hydrochloric acid and water
  5. dry with materialThe organic layer was dried with sodium sulfate
  6. concentrationconcentrated
  7. customto give a white solid

출처 및 근거

ORD 기록
ord-dd962719fdbd4bd0bc96e9960a153395
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157455B2

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