Hydrochloric Acid → HCID 22397507, 화합물

HRID 349756

반응식

HRID 349756 반응식
CCOC(/N=N/C(OCC)=O)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Cl:32][C:33]1[CH:34]=[C:35]([OH:40])[CH:36]=[CH:37][C:38]=1[F:39].C(OC([N:48]1[CH2:53][CH2:52][CH:51](O)[CH2:50][CH2:49]1)=O)(C)(C)C.Cl>C1COCC1.O1CCOCC1>[Cl:32][C:33]1[CH:34]=[C:35]([CH:36]=[CH:37][C:38]=1[F:39])[O:40][CH:51]1[CH2:52][CH2:53][NH:48][CH2:49][CH2:50]1

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 11776TriphenylphosphineHCID 757903-Chloro-4-fluorophenolHCID 643502Tert-butyl 4-hydroxypiperidine-1-carboxylateHCID 5462977Diethyl azodicarboxylate

생성물 1

HCID 22397507HCID 22397507, 화합물수율 105.2%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 312751,4-Dioxane용매

실험 절차

DEAD (0.43 ml) was added to a solution of triphenylphosphine (0.72 g), 3-chloro-4-fluorophenol (0.403 g) and 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester (0.5 g) in THF at RT. The resulting mixture was stirred overnight, HCl in dioxan (2 ml of 4M) was added and the mixture stirred at RT overnight. The mixture was then evaporated to dryness and triethylamine (5 ml) was added. The mixture was evaporated and the residue was dissolved in methanol (110 ml), placed onto a SCX cartridge (Varian, 10 g, SCX cartridge available from International Sorbent Technology Isolute® Flash SCX-2) and eluted: first with methanol then with 10% NH3 in methanol. The basic fractions were combined and evaporated to give the product as an oil (0.6 g).

후처리

  1. stirringthe mixture stirred at RT overnight
  2. customThe mixture was then evaporated to dryness and triethylamine (5 ml)
  3. additionwas added
  4. customThe mixture was evaporated
  5. dissolutionthe residue was dissolved in methanol (110 ml)
  6. washeluted
  7. customevaporated

출처 및 근거

ORD 기록
ord-80db32a74d1f4ba1a5830b7a80dae201
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179922B2

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