Pyridine → HCID 21876712, 화합물

HRID 723787노트

반응식

HRID 723787 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:15])[CH:3]=1.N1C=CC=CC=1.Cl[C:23]([O:25][CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)=[O:24]>ClCCl>[CH2:26]([O:25][C:23]([NH:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([C:9]2[CH2:14][CH2:13][S:12][CH2:11][CH:10]=2)=[C:4]([F:15])[CH:3]=1)=[O:24])[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 10387Benzyl chloroformateHCID 21876582HCID 21876582, 화합물

생성물 1

HCID 21876712HCID 21876712, 화합물수율 94.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

4-(4-Amino-2,6-difluorophenyl)-5,6-dihydro-2H-thiopyran (15.0 g, 66 mM) was dissolved in dry dichloromethane (250 ml), pyridine (9.45 g, 113 mM) added, and the whole stirred under nitrogen at −20°. Benzyl chloroformate (17.1 g, 100 mM) in dry dichloromethane (25 ml) was added dropwise, and the mixture allowed to warm to ambient over 18 hours. The mixture was washed with hydrochloric acid (1M, 2×200 ml), then brine (200 ml) and dried (magnesium sulfate). Evaporation to a small volume and dilution with isohexane gave the desired product as a white solid (22.5 g).

후처리

  1. temperatureto warm
  2. washThe mixture was washed with hydrochloric acid (1M, 2×200 ml)
  3. dry with materialbrine (200 ml) and dried (magnesium sulfate)
  4. customEvaporation to a small volume and dilution with isohexane

출처 및 근거

ORD 기록
ord-f2a168d2dbd54af38e3d5340812cfd30
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07141583B2

반응 노트

불러오는 중…