1-Propanol → 3-[4-Chloro-6-fluoro-2-propoxybenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

HRID 1419707노트

반응식

HRID 1419707 반응식
[CH2:1]([OH:4])[CH2:2][CH3:3].[H-].[Na+].Cl[C:8]1[S:9][C:10]2[C:16]([N:17]3[C:22](=[O:23])[CH:21]=[C:20]([C:24]([F:27])([F:26])[F:25])[NH:19][C:18]3=[O:28])=[C:15]([F:29])[CH:14]=[C:13]([Cl:30])[C:11]=2[N:12]=1>O1CCCC1>[Cl:30][C:13]1[C:11]2[N:12]=[C:8]([O:4][CH2:1][CH2:2][CH3:3])[S:9][C:10]=2[C:16]([N:17]2[C:22](=[O:23])[CH:21]=[C:20]([C:24]([F:26])([F:27])[F:25])[NH:19][C:18]2=[O:28])=[C:15]([F:29])[CH:14]=1

참가 물질

5

반응물 3

HCID 10311-PropanolHCID 24758Sodium hydrideHCID 109382113-[2,4-Dichloro-6-fluorobenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 153461793-[4-Chloro-6-fluoro-2-propoxybenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

108 ml of absolute n-propanol were added dropwise at room temperature to 1.1 g of sodium hydride (97% strength) in 40 ml of absolute tetrahydrofuran. Stirring was carried out for 30 minutes, after which 7.0 g of 3-[2,4-dichloro-6-fluorobenzothiazol-7-yl]-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione (compound I.4) were slowly added. Stirring was carried out for 12 hours, after which the solvent was distilled off at reduced pressure and the residue was then taken up in water. 10% strength hydrochloric acid was added to the aqueous phase until the resulting pH was from 3 to 4. The precipitate formed was separated off, washed with water and then dried. Yield: 5.2 g.

후처리

  1. stirringStirring
  2. waitwas carried out for 12 hours
  3. distillationafter which the solvent was distilled off at reduced pressure
  4. addition10% strength hydrochloric acid was added to the aqueous phase until the resulting pH
  5. customThe precipitate formed
  6. customwas separated off
  7. washwashed with water
  8. customdried

출처 및 근거

ORD 기록
ord-b22d4fb7bca04445a98ee8332890ff96
출처 데이터셋
uspto-grants-1999_03
특허 번호
US05888940

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