Acetic Acid → HCID 69907482、化合物

HRID 618132ノート

反応式

HRID 618132 の反応式
[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

参加物

7

反応物 3

HCID 176Acetic AcidHCID 167693TrimethylsilyldiazomethaneHCID 69907607HCID 69907607、化合物

生成物 1

HCID 69907482HCID 69907482、化合物

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6212Chloroform溶媒HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-edb56248339e411a8cb1935876415255
出典データセット
uspto-grants-1999_09
特許番号
US05952355

反応ノート

読み込み中…