Hydroxyamine hydrochloride → 3-Methyl-5-(1-methyl-2(S)-pyrrolidinyl)isoxazole

HRID 440085

반응식

HRID 440085 반응식
Cl.NO.C1([NH:10][C:11]([CH3:21])=[CH:12][C:13]([CH:15]2[N:19]([CH3:20])[CH2:18][CH2:17][CH2:16]2)=[O:14])CCCCC1>CO>[CH3:21][C:11]1[CH:12]=[C:13]([C@@H:15]2[CH2:16][CH2:17][CH2:18][N:19]2[CH3:20])[O:14][N:10]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 677344693-(Cyclohexylamino)-1-(1-methyl-5-pyrrolidinyl)-2-butene-1-one

생성물 1

HCID 1193803-Methyl-5-(1-methyl-2(S)-pyrrolidinyl)isoxazole

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
20 °C

실험 절차

Hydroxylamine HCl (70 mg, 1.0 mmol) was added to a solution of 3-(cyclohexylamino)-1-(1-methyl-5-pyrrolidinyl)-2-butene-1-one (160 mg, 0.64 mmol, from step 12a above) in 5 mL of methanol, and the mixture was stirred at 20±5° C. for 4 hr. The solvent was removed under vacuum at 25° C., and the residue suspended in 3 mL of water and 1 mL of H2SO4. The mixture was heated to 70° C. for 90 min, then cooled to room temperature and adjusted to pH 10 with 50% NaOH (4 g). The mixture was extracted with ethyl acetate, and the extracts were dried over Na2SO4 and concentrated. The residue was confirmed as title product by chromatographic analysis. The analytical data correspond to that given in Example 1.

후처리

  1. customThe solvent was removed under vacuum at 25° C.
  2. temperatureThe mixture was heated to 70° C. for 90 min
  3. temperaturecooled to room temperature
  4. extractionThe mixture was extracted with ethyl acetate
  5. dry with materialthe extracts were dried over Na2SO4
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5b3d197f8ad3447fb31c47426e6db5d7
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05516912

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