Triphenylphosphine → HCID 71696612, 화합물

HRID 1485837노트

반응식

HRID 1485837 반응식
[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13][CH:12]([OH:15])[CH:11]=[CH:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[F:35][C:36]1[CH:37]=[C:38]([C:42]2[CH:47]=[C:46](O)[CH:45]=[CH:44][C:43]=2[CH2:49][CH2:50][NH:51][C:52](=[O:54])[CH3:53])[CH:39]=[CH:40][CH:41]=1.CC(OC(/N=N/C(OC(C)C)=O)=O)C.C([O-])(O)=O.[Na+]>C1COCC1>[CH2:1]([O:8][CH:9]1[CH2:14][CH2:13][CH:12]([O:15][C:46]2[CH:45]=[CH:44][C:43]([CH2:49][CH2:50][NH:51][C:52](=[O:54])[CH3:53])=[C:42]([C:38]3[CH:39]=[CH:40][CH:41]=[C:36]([F:35])[CH:37]=3)[CH:47]=2)[CH:11]=[CH:10]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 5

HCID 11776TriphenylphosphineHCID 516892Sodium BicarbonateHCID 5363146Diisopropyl azodicarboxylateHCID 12827154HCID 12827154, 화합물HCID 89752224HCID 89752224, 화합물

생성물 1

HCID 71696612HCID 71696612, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 35 (70 mg, 0.34 mmol) in freshly distilled THF (3 mL) at 0° C. was added triphenyl phosphine (180 mg, 0.68 mmol) and 23 (90 mg, 0.34 mmol). DIAD (0.135 mL, 0.68 mmol) was added to the mixture dropwise. The reaction was warmed to room temperature and stirred for 4 h. The reaction mixture was treated with saturated aqueous NaHCO3 solution (2 mL), washed with water, followed by brine, dried over Na2SO4, and concentrated to give a crude mixture that was purified by column chromatography (30% 50% EtOAc in hexane) to give 36 as an oil.

후처리

  1. washwashed with water
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. customto give a crude mixture that
  5. customwas purified by column chromatography (30% 50% EtOAc in hexane)

출처 및 근거

ORD 기록
ord-66c20475096647fa82d23ebe22ab772a
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422320B2

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