Methyl iodide → HCID 20284777、化合物

HRID 127526

反応式

HRID 127526 の反応式
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]

参加物

8

反応物 5

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

生成物 1

HCID 20284777HCID 20284777、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-c88c20fec02f4ae395639a69a822b0fe
出典データセット
uspto-grants-1981_03
特許番号
US04256640

関連ノート

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