Methyl iodide → 7,9-Diethyl-3,6,7,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

HRID 840002노트

반응식

HRID 840002 반응식
[K].[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[NH:8][C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3].[CH3:21]I>CN(C)C=O>[CH2:2]([C:4]1([CH3:20])[NH:15][C:14]([CH2:17][CH3:18])([CH3:16])[CH2:13][C:6]2([NH:10][C:9](=[O:11])[N:8]([CH3:21])[C:7]2=[O:12])[CH:5]1[CH3:19])[CH3:3]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 5462222PotassiumHCID 203401897,9-Diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione2회

생성물 1

HCID 203224527,9-Diethyl-3,6,7,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To 40 ml of dimethylformamide were added 5.0 g of the potassium salt of 7,9-diethyl-6,7,9-trimethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione (Compound 1) and 11.9 g of methyl iodide; the mixture was stirred at room temperature for 16 hours. The mixture was then poured into 150 g of ice water and extracted with benzene. The benzene extract was washed with ice water and then dried over potassium carbonate. After removing the benzene, the residue was chromatographed through a column of silica gel (eluent, ethyl acetate), giving 2.7 g of Compound 2, mp 137° - 142° C.

후처리

  1. extractionextracted with benzene
  2. extractionThe benzene extract
  3. washwas washed with ice water
  4. dry with materialdried over potassium carbonate
  5. customAfter removing the benzene
  6. customthe residue was chromatographed through a column of silica gel (eluent, ethyl acetate)

출처 및 근거

ORD 기록
ord-29662d607c2444028a944f0557916ce6
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04097587

반응 노트

불러오는 중…