Acetic Acid → HCID 69907482, 화합물

HRID 618132노트

반응식

HRID 618132 반응식
[C:1]([CH2:4][S:5]/[C:6](=[CH:21]\[C:22]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[NH:24][CH:23]=1)/[C:7]([C:9]1[CH:14]=[C:13]([O:15][CH3:16])[C:12]([O:17][CH3:18])=[C:11]([O:19][CH3:20])[CH:10]=1)=[O:8])([OH:3])=[O:2].[CH3:31][Si](C=[N+]=[N-])(C)C.C(O)(=O)C>C(Cl)(Cl)Cl.CO.CCCCCC>[NH:24]1[C:25]2[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:22](/[CH:21]=[C:6](\[S:5][CH2:4][C:1]([O:3][CH3:31])=[O:2])/[C:7]([C:9]2[CH:14]=[C:13]([O:15][CH3:16])[C:12]([O:17][CH3:18])=[C:11]([O:19][CH3:20])[CH:10]=2)=[O:8])=[CH:23]1

참가 물질

7

반응물 3

HCID 176Acetic AcidHCID 167693TrimethylsilyldiazomethaneHCID 69907607HCID 69907607, 화합물

생성물 1

HCID 69907482HCID 69907482, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 6212Chloroform용매HCID 8058Hexane용매

실험 절차

Compound 107 (50.0 mg) obtained in Example 107 was dissolved in a mixed solvent of chloroform (10 ml) and methanol (5 ml), and a solution (0.5 ml) of trimethylsilyldiazomethane in hexane, followed by stirring for 10 minutes. Acetic acid (20.0 mg) was added to the reaction solution and the mixture was subjected to partitioning between chloroform and a 5% aqueous solution of sodium bicarbonate. The organic layer was concentrated under reduced pressure and the residue was purified by silica gel column chromatography. The obtained crude crystals were recrystallized from isopropyl ether to give Compound 108 (36.9 mg).

후처리

  1. customto partitioning between chloroform
  2. concentrationThe organic layer was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography
  4. customThe obtained crude crystals
  5. customwere recrystallized from isopropyl ether

출처 및 근거

ORD 기록
ord-edb56248339e411a8cb1935876415255
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952355

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