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Methyl iodide → HCID 86750226、化合物

HRID 234717
ノート
印刷プレビュー

反応式

HRID 234717 の反応式
[H-].[Na+].[C:3]1([N:9]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[C:10](=[O:30])[NH:11][NH:12][CH2:13][CH:14]2[CH2:23][CH2:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][C:20]=3[O:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])[CH2:15]2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.CI.[CH3:39]N(C)P(N(C)C)(N(C)C)=O>O1CCCC1.C(OCC)(=O)C.O>[CH3:39][N:12]([CH2:13][CH:14]1[CH2:23][CH2:22][C:21]2[C:16](=[CH:17][CH:18]=[CH:19][C:20]=2[O:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])[CH2:15]1)[NH:11][C:10]([N:9]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1)[C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)=[O:30]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6328Methyl iodideHCID 12679HexamethylphosphoramideHCID 24758Sodium hydrideHCID 86750225HCID 86750225、化合物

生成物 1

HCID 86750226HCID 86750226、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 8857Ethyl Acetate溶媒

実験手順

To a suspension of sodium hydride (6.1 mg) in tetrahydrofuran (1.5 ml) was added a solution of the compound prepared in example 15 (70 mg) in tetrahydrofuran (3 ml) under an atmosphere of argon. The mixture was stirred for 30 min at room temperature. To the mixture were successively added methyl iodide (261 mg) and hexamethylphosphoramide (1 ml), After stirred for 2 h at room temperature, the mixture was diluted with ethyl acetate and water. The mixture was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (ethyl acetate:hexane =2:3) to give the title compound (27 mg) having the following physical data.

後処理

  1. stirringAfter stirred for 2 h at room temperature
  2. extractionThe mixture was extracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materiala saturated aqueous solution of sodium chloride, successively, dried over anhydrous magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane =2:3)

出典と根拠

ORDレコード
ord-0a40a64eb5fd4534b8890b7eadef87df
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05596009

反応ノート

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