2,6-Dichlorpyridine-3-carbonyl chloride → HCID 178523747、化合物
反応式
[F:1][C:2]([F:11])([F:10])[C@H:3]1[CH2:8][CH2:7][C@H:6]([NH2:9])[CH2:5][CH2:4]1.[Cl:12][C:13]1[N:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:14]=1[C:15](Cl)=[O:16]>C1COCC1>[Cl:12][C:13]1[N:21]=[C:20]([Cl:22])[CH:19]=[CH:18][C:14]=1[C:15]([NH:9][C@H:6]1[CH2:5][CH2:4][C@H:3]([C:2]([F:10])([F:11])[F:1])[CH2:8][CH2:7]1)=[O:16]参加物
4
実験手順
A mixture of trans-4-trifluoromethyl-cyclohexylamine (4.8 g) and TEA (8.3 mL, 59.4 mmol) in THF (150 mL) is stirred for 20 min at rt. 2,6-Dichloro-nicotinoyl chloride (5.0 g, 23.8 mmol) in THF (50 mL) is added dropwise under cooling and the mixture is stirred at rt for 2 h. The reaction mixture is filtered and the filtrate is concentrated. The residue is treated with water, filtered off, washed with water and dried to give the sub-title compound.
後処理
- temperatureunder cooling
- stirringthe mixture is stirred at rt for 2 h
- filtrationThe reaction mixture is filtered
- concentrationthe filtrate is concentrated
- additionThe residue is treated with water
- filtrationfiltered off
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-af8fe419a81d4fc5b6447586c57eb546
- 出典データセット
- uspto-grants-2013_11
- 特許番号
- US08586604B2
反応ノート
読み込み中…