Iodoethane → HCID 9799580, 화합물

HRID 567063노트

반응식

HRID 567063 반응식
[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]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 9841033HCID 9841033, 화합물

생성물 1

HCID 9799580HCID 9799580, 화합물

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-70874595e67543849b090c00902e1f06
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06177449B1

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