Water → HCID 178448116、化合物

HRID 1662997ノート

反応式

HRID 1662997 の反応式
[CH:1]([C@H:4]1[CH2:9][CH2:8][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]([O:28]C)[CH:23]=3)=[N:13][N:12]=2)[CH2:6][CH2:5]1)([CH3:3])[CH3:2].C([O-])(O)=O.[Na+].O.CCOC(C)=O>C(Cl)(Cl)Cl.CO>[CH:1]([C@H:4]1[CH2:5][CH2:6][C@H:7]([NH:10][C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:14]([CH2:21][C:22]3[CH:27]=[CH:26][N:25]=[C:24]([OH:28])[CH:23]=3)=[N:13][N:12]=2)[CH2:8][CH2:9]1)([CH3:3])[CH3:2]

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 178489122HCID 178489122、化合物

生成物 1

HCID 178448116HCID 178448116、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

反応条件

温度
60 °C

実験手順

Under N2-atmosphere, 0.28 ml (2.05 mMol) Me3Sil are added to 400 mg (1.02 mMol) of trans 1-(4-isopropyl-cyclohexylamino)-4-[2-methoxy-(pyridin-4-yl)-methyl]-phthalazine in 10 ml chloroform, and the resulting mixture is stirred during 20 h at 60° C. After cooling to RT, 5 ml sat. NaHCO3-solution, 5 ml water, 20 ml EtOAc and a small amount of methanol are added, followed by agitation. The resulting white crystals are filtered off, washed with water and dried, yielding the title compound: M.p. 266-267° C. (decomposition); FAB-MS: (M+H)+=377; HPLC(Grad20-100) tRet=10.3). From the filtrate, by extraction with EtOAc, washing of the organic phase with water and brine, drying (Na2SO4), evaporation and crystallisation from dichlormethane/methanol under addition of ether, more product results.

後処理

  1. temperatureAfter cooling to RT
  2. filtrationThe resulting white crystals are filtered off
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-27dd13208ff34f13b69d588aaea49572
出典データセット
uspto-grants-2011_10
特許番号
US08034814B2

反応ノート

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