Hydrazine hydrate (1:1) → HCID 178505591, 화합물

반응식

[Cl:1][C:2]1[N:7]=[C:6](/[C:8](=[CH:18]\[N:19](C)C)/[C:9]([C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)=O)[CH:5]=[CH:4][N:3]=1.O.[NH2:23]N>>[Cl:1][C:2]1[N:7]=[C:6]([C:8]2[C:9]([C:11]3[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=3)=[N:23][NH:19][CH:18]=2)[CH:5]=[CH:4][N:3]=1

참가 물질

반응물 2

HCID 24654Hydrazine hydrate (1:1)

HCID 59038042(E)-2-(2-chloro-4-pyrimidinyl)-3-(dimethylamino)-1-(4-fluorophenyl)-2-propen-1-one

생성물 1

HCID 178505591HCID 178505591, 화합물수율 48.1%

실험 절차

A solution of the compound prepared in step 3 (4.4 g) and hydrazine hydrate (0.82 g, 0.014 mol) was stirred at room temperature for 6 hours. The yellow precipitate was collected by filtration and air-dried to give 1.85 g of 2-chloro-4-[3-(4-fluorophenyl)-1H-pyrazol-4-yl]pyrimidine as a yellow solid, mp: 204-205° C.; Anal. Calc'd for C13H8ClFN4: C, 56.84; H, 2.94; N, 20.40; Cl, 12.91. Found: C, 56.43; H, 2.76; N, 20.02; Cl, 12.97.

후처리

filtrationThe yellow precipitate was collected by filtration
customair-dried

출처 및 근거

ORD 기록: ord-71468baf794b49d68e0a1e7f56e466e2
출처 데이터셋: uspto-grants-2003_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06617324B1

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