Diisopropylethylamine → HCID 86675758、化合物
反応式
[Cl:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=O)=[C:4]([F:12])[CH:3]=1.C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.C[N+](C)=C(N(C)C)ON1C2N=CC=CC=2N=N1.[F:46][CH:47]([F:50])[CH2:48][NH2:49]>ClCCCl.ClC(Cl)C>[Cl:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([NH:49][CH2:48][CH:47]([F:50])[F:46])=[O:8])=[C:4]([F:12])[CH:3]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 4-chloro-2,5-difluorobenzoic acid (1.28 g, 6.64 mmol), N,N-diisopropylethylamine (3.5 mL, 20 mmol), and N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (3.07 g, 8.07 mmol) in 1,2-dichloroethane (20 mL) was stirred for 10 min. at room temperature prior to the addition of a solution of 2,2-difluoroethanamine (538 mg, 6.64 mmol) in dichloroethane (2 mL). The resulting solution was stirred for 1 h. at room temperature. LCMS data indicated that the major reaction component was the desired product. The crude reaction mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with methanol in dichloromethane (0-10%) to afford the desired product. LCMS (M+H)+: m/z=256.0.
出典と根拠
- ORDレコード
- ord-6a00512fdd934978984a21c00bca279e
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09023840B2
反応ノート
読み込み中…