Water → (5-chloro-1,3-dimethyl-1H-pyrazol-4-yl)methanamine hydrochloride

HRID 530794노트

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HRID 530794 반응식
[N:1]([CH2:4][C:5]1[C:6]([CH3:12])=[N:7][N:8]([CH3:11])[C:9]=1[Cl:10])=[N+]=[N-].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.O.[NH4+].[OH-]>C1COCC1>[ClH:10].[Cl:10][C:9]1[N:8]([CH3:11])[N:7]=[C:6]([CH3:12])[C:5]=1[CH2:4][NH2:1]

참가 물질

6

반응물 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 14923Ammonium HydroxideHCID 613734544-(azidomethyl)-5-chloro-1,3-dimethyl-1H-pyrazole

생성물 1

HCID 90419183(5-chloro-1,3-dimethyl-1H-pyrazol-4-yl)methanamine hydrochloride

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of compound 3 (175 mg, 0.95 mmol) in THF (5 mL) was added PPh3 (248 mg, 0.95 mmol) at 0° C. After stirring for 1 hr, water (0.03 mL) and NH4OH (0.07 mL) were added sequentially and the resulting mixture was stirred at room temperature for overnight. After the solvent was evaporated, the residue was purified with reversed flash to give a white solid. LCMS (ESI) m/z=160 (M+H)+.

후처리

  1. stirringthe resulting mixture was stirred at room temperature for overnight
  2. customAfter the solvent was evaporated
  3. customthe residue was purified with reversed flash
  4. customto give a white solid

출처 및 근거

ORD 기록
ord-db7c4232359642ff99323cbe14e94601
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353104B2

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