Hydroxyamine hydrochloride → HCID 96133985, 화합물

HRID 1752651노트

반응식

HRID 1752651 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][C:7]([C:11]#[N:12])=[CH:8][CH:9]=2)[CH:4]=[N:3]1.Cl.[NH2:14][OH:15].C(=O)(O)[O-].[Na+]>CO>[OH:15][N:14]=[C:11]([C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[N:2]([CH3:1])[N:3]=[CH:4]2)[NH2:12]

참가 물질

5

반응물 3

HCID 443297Hydroxyamine hydrochlorideHCID 516892Sodium BicarbonateHCID 105830411-Methyl-1H-indazole-5-carbonitrile

생성물 1

HCID 96133985HCID 96133985, 화합물수율 70.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1-methyl-1H-indazole-5-carbonitrile (205 mg, 1.304 mmol), hydroxylamine hydrochloride (363 mg, 5.22 mmol) and sodium bicarbonate (548 mg, 6.52 mmol) in Methanol (6 mL) was heated to 60 degrees for 90 min. The reaction mixture was cooled to ambient temperature and partitioned between EtOAc and water. The aqueous layer was extracted with EtOAc, and the combined organics washed with brine, dried (Na2SO4) and concentrated to afford the crude N′-hydroxy-1-methyl-1H-indazole-5-carboximidamide (174 mg, 0.915 mmol, 70% yield). 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 1.15-1.38 (m, 6H) 2.13 (s, 3H) 4.18 (dq, J=19.59, 7.15 Hz, 4H) 4.98 (br. s., 1H) 8.90 (br. s., 1H). LC/MS (m/z) ES+=191 (M+1).

후처리

  1. custompartitioned between EtOAc and water
  2. extractionThe aqueous layer was extracted with EtOAc
  3. washthe combined organics washed with brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ca46f6592b4c4a6a8a20ad9679b01fbb
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09163023B2

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