Diisopropylethylamine → HCID 178513419, 화합물

HRID 273179노트

반응식

HRID 273179 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178513419HCID 178513419, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-46b255942eab44d7811461e575d1c3b7
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07456210B2

반응 노트

불러오는 중…