2-(Dimethylamino)ethanol → 2-[3-(2-Dimethylaminoethoxy)propyl]-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

HRID 2351004노트

반응식

HRID 2351004 반응식
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][OH:5].[H-].[Na+].Br[CH2:10][CH2:11][CH2:12][CH:13]1[S:17][C:16]2[C:18]([CH3:28])=[C:19]([O:24][CH2:25][O:26][CH3:27])[C:20]([CH3:23])=[C:21]([CH3:22])[C:15]=2[O:14]1>CS(C)=O>[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][O:5][CH2:10][CH2:11][CH2:12][CH:13]1[S:17][C:16]2[C:18]([CH3:28])=[C:19]([O:24][CH2:25][O:26][CH3:27])[C:20]([CH3:23])=[C:21]([CH3:22])[C:15]=2[O:14]1

참가 물질

5

반응물 3

HCID 79022-(Dimethylamino)ethanolHCID 24758Sodium hydrideHCID 148021932-(3-Bromopropyl)-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

생성물 1

HCID 148021942-[3-(2-Dimethylaminoethoxy)propyl]-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

반응 조건

온도
50 °C

실험 절차

740 mg of 2-dimethylaminoethanol were dissolved in 10 ml of dimethyl sulfoxide, and 220 mg of a 50% w/w oily suspension of sodium hydride was added to the resulting solution; the reaction mixture was then heated at 50° C. for 1 hour, after which it was cooled down with ice, and a solution of 1.68 g of 2-(3-bromopropyl)-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 87) in 5 ml of dimethyl sulfoxide was added dropwise, while stirring. The reaction product was then subjected to the same reaction process, extraction and separation procedures as described in (a) above, to give the title compound with the same Rf value and mass spectrum as those of the product obtained in (a).

후처리

  1. additionwas added to the resulting solution
  2. temperatureafter which it was cooled down with ice
  3. extractionThe reaction product was then subjected to the same reaction process, extraction and separation procedures

출처 및 근거

ORD 기록
ord-919d7175fcdf485cacaea0bc701bd68c
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871762

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