Ether hydrochloride → cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochloride

HRID 1269937노트

반응식

HRID 1269937 반응식
[ClH:1].C(OCC)C.[CH2:7]([O:10][C:11]1[C:19]([O:20][C@@H:21]2[CH2:26][CH2:25][CH2:24][C@H:23]([NH2:27])[CH2:22]2)=[CH:18][CH:17]=[C:16]2[C:12]=1[CH:13]=[N:14][NH:15]2)[CH2:8][CH3:9]>CO>[ClH:1].[CH2:7]([O:10][C:11]1[C:19]([O:20][C@@H:21]2[CH2:26][CH2:25][CH2:24][C@H:23]([NH2:27])[CH2:22]2)=[CH:18][CH:17]=[C:16]2[C:12]=1[CH:13]=[N:14][NH:15]2)[CH2:8][CH3:9]

참가 물질

4

반응물 2

HCID 10953452Ether hydrochlorideHCID 69432506cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine

생성물 1

HCID 69433087cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochloride수율 83%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Under a nitrogen atmosphere, 1M-hydrochloric acid-diethyl ether (341 μl, 0.341 mmol) was added dropwise to a solution of cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine (82.3 mg, 0.284 mmol) in methanol (2 ml) at room temperature. After 1 hour, the mixture thus obtained was concentrated under reduced pressure and the resulting residue was crystallized from ethyl acetate, followed by filtration under reduced pressure, and then drying. The solid thus obtained was washed with hexane by repulping to obtain cis-3-[(4-propoxy-1H-indazol-5-yl)oxy]cyclohexanamine hydrochloride (76.8 mg, 83%).

후처리

  1. customthe mixture thus obtained
  2. concentrationwas concentrated under reduced pressure
  3. customthe resulting residue was crystallized from ethyl acetate
  4. filtrationfollowed by filtration under reduced pressure
  5. customdrying
  6. customThe solid thus obtained
  7. washwas washed with hexane

출처 및 근거

ORD 기록
ord-8d7aa124532f48b88a2e8567996019fe
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

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