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Triphenylphosphine → HCID 71681343, 화합물

HRID 929897
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HRID 929897 반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[Br:20]Br.[C:22]([O:26][C:27]([C@:29]1([NH:43][C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:34][C@H:33](O)[C@@H:32]2[C@H:30]1[C@H:31]2[C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])=[O:28])([CH3:25])([CH3:24])[CH3:23]>C1(C)C=CC=CC=1.N1C=CC=CC=1.C(OCC)(=O)C>[C:22]([O:26][C:27]([C@:29]1([NH:43][C:44]([O:46][C:47]([CH3:50])([CH3:49])[CH3:48])=[O:45])[CH2:34][C@@H:33]([Br:20])[C@@H:32]2[C@H:30]1[C@H:31]2[C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])=[O:28])([CH3:25])([CH3:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11776TriphenylphosphineHCID 24408BromineHCID 59712892ditert-butyl(1S,2S,4S,5R,6R)-2-(tert-butoxycarbonylamino)-4-hydroxy-bicyclo[3.1.0]hexane-2,6-dicarboxylate

생성물 1

HCID 71681343HCID 71681343, 화합물수율 78.2%

시약·촉매·용매 3

HCID 1049Pyridine용매
HCID 1140
Toluene
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

Dissolve triphenylphosphine (41.97 g, 158.4 mmol) in fresh toluene (660 mL) and add bromine (8.14 mL, 158.4 mmol) until a yellow color persists. Add dropwise a solution of ditert-butyl(1S,2S,4S,5R,6R)-2-(tert-butoxycarbonylamino)-4-hydroxy-bicyclo[3.1.0]hexane-2,6-dicarboxylate (32.75 g, 79.2 mmol) in toluene (176 mL) and anhydrous pyridine (528 mL) during 45 min. Stir the reaction at 75° C. overnight. Cool to room temperature, dilute with ethyl acetate, filter and concentrate to dryness. Slurry the crude in methyl tert-butyl ether, filter to remove the solids and concentrate the filtrate to dryness. Purify the crude by silica gel chromatography (750 g) eluting with hexane:ethyl acetate (0:100 to 80:20) to obtain the title compound as a white solid (29.52 g, 78%). MS (m/z): 498, 500 (M+23).

후처리

  1. customthe reaction at 75° C. overnight
  2. filtrationfilter
  3. concentrationconcentrate to dryness
  4. filtrationfilter
  5. customto remove the solids
  6. concentrationconcentrate the filtrate to dryness
  7. customPurify the crude by silica gel chromatography (750 g)
  8. washeluting with hexane:ethyl acetate (0:100 to 80:20)

출처 및 근거

ORD 기록
ord-b158deb98977420782a46409727c1b87
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296710B2

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