Acetic Acid → HCID 69545831, 화합물

HRID 2086254노트

반응식

HRID 2086254 반응식
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:13][CH2:12][N:11]([N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)[CH2:17][CH2:16]2)[C:10]1=[O:27])=[O:7])([CH3:4])([CH3:3])[CH3:2].C(O)(=O)C.C([BH3-])#N.[Na+]>CO>[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:13][CH2:12][N:11]([NH:14][CH:15]2[CH2:16][CH2:17][N:18]([C:21]3[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=3)[CH2:19][CH2:20]2)[C:10]1=[O:27])=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 5003444Sodium cyanoborohydrideHCID 69545990(3S)-3-(tert-butoxycarbonylamino)-1-[1-(4-pyridyl)-4-piperidinylideneamino]-2-pyrrolidone

생성물 1

HCID 69545831HCID 69545831, 화합물수율 71.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

(3S)-3-(tert-Butoxycarbonylamino)-1-[1-(4-pyridyl)-4-piperidinylideneamino]-2-pyrrolidone (3.57 g) was dissolved in methanol (40 ml), combined with acetic acid (2.05 g) with cooling on ice, followed by sodium cyanoborohydride (807 mg) and stirred at room temperature for 30 minutes. The reaction mixture was concentrated, and the residue was combined with an aqueous solution of sodium hydroxide, extracted with dichloromethane, dried, concentrated, and purified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1) to obtain the title compound (2.56 g) as a colorless amorphous material.

후처리

  1. temperaturewith cooling on ice
  2. concentrationThe reaction mixture was concentrated
  3. extractionextracted with dichloromethane
  4. customdried
  5. concentrationconcentrated
  6. custompurified by a column chromatography (dichloromethane: 10% aqueous ammonia-containing methanol=20:1)

출처 및 근거

ORD 기록
ord-813ac87904194d809ac3afa2643898db
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06723722B1

반응 노트

불러오는 중…