Water → HCID 86628297, 화합물

HRID 21265노트

반응식

HRID 21265 반응식
[CH3:1][S:2]([O:5][C:6]1[C:14]([CH:15](OC)[O:16][CH3:17])=[CH:13][C:12]([I:20])=[C:11]2[C:7]=1[CH:8](OC)[N:9](C(C)(C1C=CC=CC=1)C)[C:10]2=[O:21])(=[O:4])=[O:3].FC(F)(F)C(O)=O.C([SiH](CC)CC)C.O>[N+](C)([O-])=O.CCCCCC.C(OCC)(=O)C>[CH3:1][S:2]([O:5][C:6]1[C:14]([CH2:15][O:16][CH3:17])=[CH:13][C:12]([I:20])=[C:11]2[C:7]=1[CH2:8][NH:9][C:10]2=[O:21])(=[O:3])=[O:4]

참가 물질

8

반응물 4

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 866282964-Methanesulfonyloxy-5-dimethoxymethyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone

생성물 1

HCID 86628297HCID 86628297, 화합물수율 72.4%

시약·촉매·용매 3

HCID 6375Nitromethane용매HCID 8058Hexane용매HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

In a similar manner to Step 4 of Example 16, 4-methanesulfonyloxy-5-dimethoxymethyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (226 mg, 0.393 mmol) was dissolved in nitromethane (5 mL), and the solution was added with trifluoroacetic acid (0.775 mL, 10.1 mmol) and triethylsilane (0.406 mL, 2.51 mmol), followed by stirring at 50° C. for 1 hour. The reaction mixture was added with water, ethyl acetate and hexane. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure to obtain 4-methanesulfonyloxy-5-methoxymethyl-7-iodoisoindolinone (113 mg, yield 72%).

후처리

  1. filtrationThe precipitated solid was collected by filtration
  2. washwashed with water
  3. customby drying under reduced pressure

출처 및 근거

ORD 기록
ord-576ef63e032743879434c13e7bc63fbb
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745641B2

반응 노트

불러오는 중…