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Ammonia → 6-chloro-4-(1-methyl-1H-pyrazol-3-ylamino)-pyridazine-3-carboxylic acid amide

HRID 1396353
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반응식

HRID 1396353 반응식
C[O:2][C:3]([C:5]1[N:6]=[N:7][C:8]([Cl:18])=[CH:9][C:10]=1[NH:11][C:12]1[CH:16]=[CH:15][N:14]([CH3:17])[N:13]=1)=O.[NH3:19]>CO>[Cl:18][C:8]1[N:7]=[N:6][C:5]([C:3]([NH2:19])=[O:2])=[C:10]([NH:11][C:12]2[CH:16]=[CH:15][N:14]([CH3:17])[N:13]=2)[CH:9]=1
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 86689721HCID 86689721, 화합물

생성물 1

HCID 866897226-chloro-4-(1-methyl-1H-pyrazol-3-ylamino)-pyridazine-3-carboxylic acid amide수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6-Chloro-4-(1-methyl-1H-pyrazol-3-ylamino)-pyridazine-3-carboxylic acid methyl ester (75 mg, 0.28 mmol) was suspended in 7M ammonia in methanol (3 mL). After 16 h, the reaction mixture was concentrated in vacuo to give 6-chloro-4-(1-methyl-1H-pyrazol-3-ylamino)-pyridazine-3-carboxylic acid amide (70 mg, 100%) as an off-white solid which was used directly in the next step without purification. 1H NMR (300 MHz, DMSO-d6) δ ppm 11.39 (s, 1H) 8.77 (br. s., 1H) 8.24 (s, 1H) 8.13 (br. s., 1H) 7.72 (d, J=2.3 Hz, 1H) 6.18 (d, J=2.3 Hz, 1H) 3.84 (s, 3H); LCMS (EI/CI) m/z: 253 [M+H].

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo

출처 및 근거

ORD 기록
ord-5bf733292c25497e90b2ebb81508d5bc
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901124B2

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