Hydrochloric Acid → HCID 10888841, 화합물

HRID 892807노트

반응식

HRID 892807 반응식
C1([C@H](N)C)C=CC=CC=1.[F:10][C:11]1[CH:16]=[CH:15][C:14]([CH:17]([CH:21]([CH3:23])[CH3:22])[C:18]([OH:20])=[O:19])=[CH:13][CH:12]=1.Cl>C(#N)C.CCOCC>[F:10][C:11]1[CH:12]=[CH:13][C:14]([C@@H:17]([CH:21]([CH3:23])[CH3:22])[C:18]([OH:20])=[O:19])=[CH:15][CH:16]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 6431891-Phenethylamine, (+)-HCID 98005182-(4-Fluorophenyl)-3-methylbutanoic acid

생성물 1

HCID 10888841HCID 10888841, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6342Acetonitrile용매2회

실험 절차

A solution of 63.0 g (0.52 mol) of [R]-(+)-1-phenylethylamine in 800 ml of acetonitrile was added with stirring to a solution of 204.1 g (1.04 mol) of rac. 2-(p-fluorophenyl)-3-methylbutyric acid in 1200 ml of acetonitrile. After 1 hour the crystalline precipitate was filtered off, washed with 300 ml of acetonitrile and dried overnight under reduced pressure at 50°. After repeated recrystallization from ethanol, the corresponding salt was obtained as colorless crystals, m.p. 209°-210°. The salt was suspended in ether and treated with 3N hydrochloric acid to pH 1. The ethereal solution was washed with water, dried and evaporated under reduced pressure, yielding [R]-(-)-2-(p-fluorophenyl)-3-methylbutyric acid, m.p. 56°-57°; [α]D20 =-48.4° (c=1, methanol).

후처리

  1. filtrationAfter 1 hour the crystalline precipitate was filtered off
  2. washwashed with 300 ml of acetonitrile
  3. customdried overnight under reduced pressure at 50°
  4. customrecrystallization from ethanol
  5. customthe corresponding salt was obtained as colorless crystals, m.p. 209°-210°
  6. washThe ethereal solution was washed with water
  7. customdried
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3b9fc2b7b3da452d813ae583862aa451
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05120759

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