Methyl iodide → HCID 20284777, 화합물

HRID 127526

반응식

HRID 127526 반응식
C[Mg]I.[Mg].[CH3:5]I.[CH:7]([CH:9]1[C:21]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[NH:14][C:13]=2[S:12][CH2:11][CH2:10]1)=[O:8].[Cl-].[NH4+]>CCOCC.C1C=CC=CC=1>[OH:8][CH:7]([CH:9]1[C:21]2[C:20]3[C:15](=[CH:16][CH:17]=[CH:18][CH:19]=3)[NH:14][C:13]=2[S:12][CH2:11][CH2:10]1)[CH3:5]

참가 물질

8

반응물 5

HCID 6328Methyl iodideHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 147356294-Formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indoleHCID 178418373HCID 178418373, 화합물

생성물 1

HCID 20284777HCID 20284777, 화합물

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 3283Diethyl Ether용매

실험 절차

Methyl magnesium iodide prepared from reaction of magnesium (2.4 g) and methyl iodide (13.9 g) in absolute ether is dissolved in absolute benzene (50 ml) and a solution of 4-formyl-2,3,4,9-tetrahydrothiopyrano[2,3-b]indole (5.5 g) in absolute benzene (60 ml) is added dropwise thereto during 3 hours. The mixture is stirred at room temperature for 1 hour, poured slowly into an ice water containing ammonium chloride (10 g) and extracted with ether. The extract is evaporated. The oily residue is chromatographed on a column of silica gel and eluted with ether-benzene (1:50). The eluate is evaporated. The residue is again chromatographed on a column of silica gel and eluted with benzene and ether-benzene (1:20). The title compound is obtained from the latter eluate as an oil (4.58 g).

후처리

  1. extractionextracted with ether
  2. customThe extract is evaporated
  3. customThe oily residue is chromatographed on a column of silica gel
  4. washeluted with ether-benzene (1:50)
  5. customThe eluate is evaporated
  6. customThe residue is again chromatographed on a column of silica gel
  7. washeluted with benzene and ether-benzene (1:20)

출처 및 근거

ORD 기록
ord-c88c20fec02f4ae395639a69a822b0fe
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256640

연결된 노트

불러오는 중…