Ethanol hydrochloride → 2-Cyclopropyl-7-[(3s)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile hydrochloride

HRID 17462

反応式

HRID 17462 の反応式
[CH:1]1([C:4]2[O:5][C:6]3[C:7](=[C:9]([C:24]#[N:25])[C:10]([CH3:23])=[C:11]([CH:21]=[O:22])[C:12]=3[N:13]3[CH2:17][CH2:16][C@H:15]([N:18]([CH3:20])[CH3:19])[CH2:14]3)[N:8]=2)[CH2:3][CH2:2]1.[ClH:26].C(O)C>C(O)C.C(OCC)C>[ClH:26].[CH:1]1([C:4]2[O:5][C:6]3[C:7](=[C:9]([C:24]#[N:25])[C:10]([CH3:23])=[C:11]([CH:21]=[O:22])[C:12]=3[N:13]3[CH2:17][CH2:16][C@H:15]([N:18]([CH3:20])[CH3:19])[CH2:14]3)[N:8]=2)[CH2:2][CH2:3]1

参加物

5

反応物 2

HCID 21887872Ethanol hydrochlorideHCID 866308522-Cyclopropyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile

生成物 1

HCID 875066112-Cyclopropyl-7-[(3s)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile hydrochloride

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

The above-obtained 2-cyclopropyl-7-[(3S)-3-(dimethylamino)pyrrolidin-1-yl]-6-formyl-5-methyl-1,3-benzoxazole-4-carbonitrile (50 mg, 0.15 mmol) was dissolved in ethanol (0.5 ml) and diethyl ether (1 ml), then at room temperature, 1 mol hydrochloric acid/ethanol solution (162 μl, 0.16 mmol) was added. After stirring under nitrogen atmosphere at the same temperature for 3 hours, the solvent was evaporated away under reduced pressure. Diethyl ether was added to the residue, and this was concentrated under reduced pressure. This operation was repeated further twice.

後処理

  1. customthe solvent was evaporated away under reduced pressure
  2. additionDiethyl ether was added to the residue
  3. concentrationthis was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-2a61c6f12b354501a8bb69fbf7daa579
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

関連ノート

読み込み中…