4-Hydroxybenzophenone → HCID 89906737, 화합물

HRID 531395

반응식

HRID 531395 반응식
[OH:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:7])=[CH:4][CH:3]=1.[H-].[Na+].Br[CH2:19][C:20]1([CH2:24][OH:25])[CH2:23][O:22][CH2:21]1.BrCC(CBr)(CO)CO>C1COCC1>[OH:25][CH2:24][C:20]1([CH2:19][O:1][C:2]2[CH:3]=[CH:4][C:5]([C:6]([C:8]3[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=3)=[O:7])=[CH:14][CH:15]=2)[CH2:23][O:22][CH2:21]1

참가 물질

6

반응물 4

HCID 143474-HydroxybenzophenoneHCID 186922,2-Bis(bromomethyl)-1,3-propanediolHCID 24758Sodium hydrideHCID 529264[3-(Bromomethyl)oxetan-3-yl]methanol

생성물 1

HCID 89906737HCID 89906737, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

Dissolve 4-hydroxybenzophenone in anhydrous THF and treat it with equimolar quantity of sodium hydride at 0° C. for 2 h. Stir and warm the suspension to 50° C. and treat it with an equimolar quantity of 3-Bromomethyl-3-hydroxymethyloxetane (readily prepared in one step by method described in U.S. Pat. No. 5,489,700 or Tet. Lett. 2011, 52, p. 565-567 from commercially available 2,2-bis-(bromomethyl)propane-1,3-diol). Stir overnight at 50° C., filter the reaction mixture, evaporate the filtrate to dryness and purify the residue by column chromatography to provide (4-{[3-(hydroxymethyl)oxetan-3-yl]methoxy}phenyl)(phenyl)methanone.

후처리

  1. customreadily prepared in one step by method
  2. stirringStir overnight at 50° C.
  3. filtrationfilter the reaction mixture
  4. customevaporate the filtrate to dryness
  5. custompurify the residue by column chromatography

출처 및 근거

ORD 기록
ord-96ea51ed7379461cb89c0e2a7f1e00f0
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09353211B2

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