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

HRID 530794ノート

反応式

HRID 530794 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-db7c4232359642ff99323cbe14e94601
出典データセット
uspto-grants-2016_05
特許番号
US09353104B2

反応ノート

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