Acetic Acid → HCID 68130945, 화합물

HRID 1287644노트

반응식

HRID 1287644 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:23])[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH:16]=[C:15]([C:18]3OC=C[N:22]=3)[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[Cr](O)(O)(=O)=O.C(=O)([O-])[O-].[Na+].[Na+].Cl.[C:36](O)(=[O:38])[CH3:37]>CO.CCOCC>[O:38]1[CH:36]=[CH:37][C:18]([C:15]2[CH2:14][CH2:13][N:12]([CH2:11][CH2:10][CH2:9][C:8]([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)=[O:23])[CH2:17][CH:16]=2)=[N:22]1

참가 물질

8

반응물 5

HCID 176Acetic Acid2회HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 24425Chromic AcidHCID 21505599HCID 21505599, 화합물

생성물 1

HCID 68130945HCID 68130945, 화합물

시약·촉매·용매 2

HCID 887Methanol촉매HCID 3283Diethyl Ether용매

실험 절차

A 1.58 g. portion of 3,6-dihydro-α-(p-fluorophenyl)- 4-(2-oxazolyl)-1(2H)-pyridinebutanol, prepared as described in Example 15, in 45 ml. of acetic acid is stirred at room temperature. A 30 ml. portion of chromic acid in acetic acid is added dropwise. The mixture is stirred for 2 hours and allowed to stand overnight. A few drops of methanol are added, the mixture is poured into ice water and neutralized with sodium carbonate. The mixture is extracted with ether. The ether extract is dried over magnesium sulfate, filtered and evaporated yielding an oil which solidifies. This solid is dissolved in ether, alcoholic HCl is added and the mixture is filtered. The solid is slurried in acetone, filtered and recrystallized twice from ethanol, m.p. 178°-178.5° C.

후처리

  1. waitto stand overnight
  2. extractionThe mixture is extracted with ether
  3. extractionThe ether extract
  4. dry with materialis dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customyielding an oil which
  8. filtrationthe mixture is filtered
  9. filtrationfiltered
  10. customrecrystallized twice from ethanol, m.p. 178°-178.5° C.

출처 및 근거

ORD 기록
ord-35dc9d50eab24fa0b440a732fed1ed25
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03985754

반응 노트

불러오는 중…