1-Hydroxybenzotriazole → 2-Chloro-6-(cyclopropylacetyl)-5,6,7,8-tetrahydro-1,6-naphthyridine
反応式
[CH:1]1([CH2:4][C:5]([OH:7])=O)[CH2:3][CH2:2]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1.Cl.[Cl:43][C:44]1[CH:53]=[CH:52][C:51]2[CH2:50][NH:49][CH2:48][CH2:47][C:46]=2[N:45]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[Cl:43][C:44]1[CH:53]=[CH:52][C:51]2[CH2:50][N:49]([C:5](=[O:7])[CH2:4][CH:1]3[CH2:2][CH2:3]3)[CH2:48][CH2:47][C:46]=2[N:45]=1参加物
7
反応物 5
生成物 1
試薬・触媒・溶媒 1
実験手順
To a stirred solution of cyclopropylacetic acid (24 mg, 0.24 mmol) in DMF (1 ml) at room temperature was added HBTU (185 mg, 0.49 mmol) and HOBt (72 mg, 0.53 mmol) sequentially and the resulting solution stirred for 15 mins. 2-Chloro-5,6,7,8-tetrahydro-1,6-naphthyridine hydrochloride (50 mg, 0.24 mmol) and DIPEA (89 μl, 0.53 mmol) in DMF (1 ml) were then added and the resulting mixture stirred at room temperature for 16 hours. The reaction mixture was evaporated to dryness and the residue was purified by FCC on silica gel (99:1:1 DCM/MeOH/NH3) to provide the title compound (56 mg, 95%).
後処理
- stirringthe resulting mixture stirred at room temperature for 16 hours
- customThe reaction mixture was evaporated to dryness
- customthe residue was purified by FCC on silica gel (99:1:1 DCM/MeOH/NH3)
出典と根拠
- ORDレコード
- ord-9705bd990e90403ea3ccc976deb7db88
- 出典データセット
- uspto-grants-2014_04
- 特許番号
- US08691804B2
反応ノート
読み込み中…