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

HRID 1269937ノート

反応式

HRID 1269937 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-8d7aa124532f48b88a2e8567996019fe
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

反応ノート

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