Diethylaminopropyl chloride, hydrochloride → HCID 21264536, 화합물

HRID 567077노트

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HRID 567077 반응식
[CH3:1][C:2]1([CH3:19])[CH2:11][CH:10]([N:12]([CH3:17])[S:13]([CH3:16])(=[O:15])=[O:14])[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([OH:18])[CH:8]=2)[O:3]1.Cl.[CH2:21]([N:23]([CH2:26][CH2:27][CH2:28]Cl)[CH2:24][CH3:25])[CH3:22]>CN(C=O)C.CC(=O)OCC>[CH2:21]([N:23]([CH2:24][CH3:25])[CH2:26][CH2:27][CH2:28][O:18][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[O:3][C:2]([CH3:19])([CH3:1])[CH2:11][CH:10]2[N:12]([CH3:17])[S:13]([CH3:16])(=[O:15])=[O:14])[CH3:22]

참가 물질

5

반응물 2

HCID 145749Diethylaminopropyl chloride, hydrochlorideHCID 21264510HCID 21264510, 화합물

생성물 1

HCID 21264536HCID 21264536, 화합물수율 48.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

0.7g (2.5 mmol) of N-[2,2-dimethyl-6-hydroxychroman-4-yl]-N-methylmethanesulfonamide (Example 15b) was stirred at RT for 1 h with 1.6 g (5.2 mmol) of phosphazene base [tert-butylimino-tri(pyrrolidino)phosphorane] in 2.5 ml of DMF. 0.48 g (2.6 mmol) of diethylaminopropyl chloride hydrochloride was then added and the mixture was heated to 100° C. for 8 h. After stripping off the solvent in vacuo, the residue was taken up in EA and the mixture was washed with water. After drying over magnesium sulfate and chromatography through a short silica gel column, 0.48 g of N-[6-(3-diethylaminopropoxy)-2,2-dimethylchroman-4-yl]-N-methylmethanesulfonamide was obtained as a glassy solid.

후처리

  1. washthe mixture was washed with water
  2. dry with materialAfter drying over magnesium sulfate and chromatography through a short silica gel column

출처 및 근거

ORD 기록
ord-25179f47bb974260b619b11519bb55fb
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06177449B1

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