Diisopropylethylamine → HCID 178513419、化合物

HRID 273179ノート

反応式

HRID 273179 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:21]=[CH:22][CH:23]=1)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:17](=[O:18])[CH2:16][C@@H:15]([C:19]#[N:20])[CH2:14]2)=[CH:9][CH:8]=1.Cl.[NH2:25][OH:26].C(N(CC)C(C)C)(C)C>C(O)C>[F:1][C:2]1[CH:3]=[C:4]([CH:21]=[CH:22][CH:23]=1)[CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:17](=[O:18])[CH2:16][C@@H:15]([C:19]([NH:25][OH:26])=[NH:20])[CH2:14]2)=[CH:9][CH:8]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 443297Hydroxyamine hydrochlorideHCID 69309400(R)-1-[4-(3-Fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carbonitrile

生成物 1

HCID 178513419HCID 178513419、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

(R)-1-[4-(3-Fluoro-benzyloxy)-phenyl]-5-oxo-pyrrolidine-3-carbonitrile (0.211 g, 0.001 mol) and hydroxylamine hydrochloride (0.047 g, 0.001 mol) were dissolved in ethanol (4 ml) and N,N-diisopropylethylamine (0.120 ml, 0.001 mol) was added. The reaction mixture was stirred under reflux for three hours. The reaction was cooled to room temperature, the solvent was evaporated and the residue extracted with dichloromethane and purified by column chromatography on silica gel using a 19:1-mixture of dichloromethane and methanol as the eluent to yield (0.220 g, 94% of theory) of a yellow oil. MS (m/e)=344.3(M+H)+.

後処理

  1. temperatureunder reflux for three hours
  2. customthe solvent was evaporated
  3. extractionthe residue extracted with dichloromethane
  4. custompurified by column chromatography on silica gel using a 19
  5. custom1-mixture of dichloromethane and methanol as the eluent to yield (0.220 g, 94% of theory) of a yellow oil

出典と根拠

ORDレコード
ord-46b255942eab44d7811461e575d1c3b7
出典データセット
uspto-grants-2008_11
特許番号
US07456210B2

反応ノート

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