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Methyl iodide → HCID 86750226, 화합물

HRID 234717
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HRID 234717 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6328Methyl iodideHCID 12679HexamethylphosphoramideHCID 24758Sodium hydrideHCID 86750225HCID 86750225, 화합물

생성물 1

HCID 86750226HCID 86750226, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-0a40a64eb5fd4534b8890b7eadef87df
출처 데이터셋
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05596009

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