76700-85-1 → HCID 20202839, 화합물

HRID 544577노트

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HRID 544577 반응식
[F:1][C:2]([F:12])([F:11])[CH2:3][NH:4][C:5]([NH:7][C:8]([NH2:10])=[S:9])=[NH:6].Cl[CH2:14][C:15](=O)[CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20]>CCO>[F:12][C:2]([F:1])([F:11])[CH2:3][N:4]=[C:5]([NH2:6])[NH:7][C:8]1[S:9][CH:14]=[C:15]([CH2:16][CH2:17][CH2:18][C:19]([O:21][CH3:22])=[O:20])[N:10]=1

참가 물질

4

반응물 2

HCID 1111662576700-85-1HCID 178512206HCID 178512206, 화합물

생성물 1

HCID 20202839HCID 20202839, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To 2,2,2-trifluoroethylamidinothiourea (2.1 g.) in hot EtOH (20 ml.) was added a solution of methyl 6-chloro-5-oxohexanoate (2.0 g.) in hot EtOH (20 ml.). The mixture was heated under reflux for 1 hour and then evaporated to dryness. The residue was partitioned between ether (20 ml.) and water (60 ml.). The aqueous layer was separated, basified with sodium bicarbonate and extracted with EtOAc. The organic layer was evaporated to dryness to give a gum which was recrystallised from EtOAc/ether/acetone to give methyl 4-[2-(2-[2,2,2-trifluoroethyl]guanidino)thiazol-4-yl]butyrate which was used without further purification.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1 hour
  3. customevaporated to dryness
  4. customThe residue was partitioned between ether (20 ml.) and water (60 ml.)
  5. customThe aqueous layer was separated
  6. extractionextracted with EtOAc
  7. customThe organic layer was evaporated to dryness
  8. customto give a gum which
  9. customwas recrystallised from EtOAc/ether/acetone

출처 및 근거

ORD 기록
ord-b6e9ce6f7c9249bcac5b934657157ae6
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04451463

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