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1,4-Dioxane → (S)-2'-(neopentyloxy)-7'-(pyridin-2-yl)-5H-spiro[oxazole-4,9'-xanthen]-2-amine

HRID 1970285
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HRID 1970285 반응식
Br[C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][C:8]([O:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:9][CH:10]=3)[C@:5]3([CH2:25][O:24][C:23]([NH2:26])=[N:22]3)[C:4]=2[CH:3]=1.C([Sn](CCCC)(CCCC)[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=1)CCC.O1CCOCC1>CS(C)=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:17]([O:16][C:8]1[CH:9]=[CH:10][C:11]2[O:12][C:13]3[C:4](=[CH:3][C:2]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][N:33]=4)=[CH:15][CH:14]=3)[C@@:5]3([CH2:25][O:24][C:23]([NH2:26])=[N:22]3)[C:6]=2[CH:7]=1)[C:18]([CH3:19])([CH3:20])[CH3:21]
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참가 물질

6

반응물 3

HCID 312751,4-DioxaneHCID 6077842-(Tributylstannyl)pyridineHCID 58466128(R)-2'-bromo-7'-(neopentyloxy)-5H-spiro[oxazole-4,9'-xanthen]-2-amine

생성물 1

HCID 58466301(S)-2'-(neopentyloxy)-7'-(pyridin-2-yl)-5H-spiro[oxazole-4,9'-xanthen]-2-amine

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물
촉매
HCID 679Dimethyl Sulfoxide용매

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온도
100 °C

실험 절차

A vial was charged with (R)-2′-bromo-7′-(neopentyloxy)-5H-spiro[oxazole-4,9′-xanthen]-2-amine (0.050 g, 0.120 mmol), tetrakis(triphenylphosphine)palladium (0) (0.014 g, 0.012 mmol), 2-(tributylstannyl)pyridine (0.132 g, 0.359 mmol), and dioxane (0.6 mL). The reaction was stirred overnight at 100° C. The mixture was diluted with DMSO and filtered through a syringe filter, which was flushed with additional DMSO. The material was purified via Gilson HPLC (10-90% MeCN:H2O). The clean product fractions were partitioned between DCM and saturated sodium bicarbonate solution. The aqueous layer was extracted with DCM, and the combined organic layers were dried with sodium sulfate, filtered, and concentrated to afford (S)-2′-(neopentyloxy)-7′-(pyridin-2-yl)-5H-spiro[oxazole-4,9′-xanthen]-2-amine as a white solid. MS MH+ 416.4

후처리

  1. filtrationfiltered through a syringe
  2. filtrationfilter
  3. customwhich was flushed with additional DMSO
  4. customThe material was purified via Gilson HPLC (10-90% MeCN:H2O)
  5. customThe clean product fractions were partitioned between DCM and saturated sodium bicarbonate solution
  6. extractionThe aqueous layer was extracted with DCM
  7. dry with materialthe combined organic layers were dried with sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b7a4396103854f13a01e13422ececc3e
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426447B2

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