Iodoethane → HCID 9799580、化合物

HRID 567063ノート

反応式

HRID 567063 の反応式
[CH2:1]([N:3]([CH:8]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([O:18][CH2:19][CH2:20][OH:21])[CH:16]=2)[O:11][C:10]([CH3:23])([CH3:22])[CH2:9]1)[S:4]([CH3:7])(=[O:6])=[O:5])[CH3:2].[H-].[Na+].[CH2:26](I)[CH3:27]>CC(N(C)C)=O>[CH2:26]([O:21][CH2:20][CH2:19][O:18][C:15]1[CH:16]=[C:17]2[C:12](=[CH:13][CH:14]=1)[O:11][C:10]([CH3:22])([CH3:23])[CH2:9][CH:8]2[N:3]([CH2:1][CH3:2])[S:4]([CH3:7])(=[O:5])=[O:6])[CH3:27]

参加物

5

反応物 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 9841033HCID 9841033、化合物

生成物 1

HCID 9799580HCID 9799580、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

2.3 g (6.7 mmol) of N-ethyl-N-[6-(2-hydroxyethoxy)-2,2-dimethylchroman-4-yl]methanesulfonamide (Example 8) were alkylated with 0.48 g (about 10 mmol) of NaH (80 percent dispersion) and 1.6 ml (about 20 mmol) of ethyl iodide in 50 ml of DMA under nitrogen. After working up and purification by column chromatography on silica gel, 1.0 g of the title compound was crystallized from corresponding fractions using petroleum ether, m.p. 73-75° C.

後処理

  1. custompurification by column chromatography on silica gel, 1.0 g of the title compound
  2. customwas crystallized from corresponding fractions

出典と根拠

ORDレコード
ord-70874595e67543849b090c00902e1f06
出典データセット
uspto-grants-2001_01
特許番号
US06177449B1

反応ノート

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