Carbon tetrabromide → HCID 11531974, 화합물

HRID 2356104노트

반응식

HRID 2356104 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=2)=[C:5]([O:19][CH3:20])[CH:4]=1)=O.[C:21](Br)(Br)([Br:23])[Br:22].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>ClCCl>[Br:22][C:21]([Br:23])=[CH:1][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([C:15]([O:17][CH3:18])=[O:16])=[CH:11][CH:10]=2)=[C:5]([O:19][CH3:20])[CH:4]=1

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 11558086Methyl 4'-formyl-2'-methoxy[1,1'-biphenyl]-4-carboxylate

생성물 1

HCID 11531974HCID 11531974, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of Example 122I (1.35 g, 5.0 mmol) in dichloromethane (30 mL) at room temperature was treated with carbon tetrabromide (1.82 g, 5.5 mmol) and triphenylphosphine (2.88 g, 11 mmol), stirred for 1 hour, treated with hexanes (50 mL), and filtered through silica gel (50 g). The solution was rinsed with 1:1 water/dichloromethane, separated, and the organic phase was concentrated. The concentrate was purified by flash column chromatography on silica gel with 2-10% ethyl acetate/hexanes to provide the desired product.

후처리

  1. filtrationfiltered through silica gel (50 g)
  2. washThe solution was rinsed with 1:1 water/dichloromethane
  3. customseparated
  4. concentrationthe organic phase was concentrated
  5. customThe concentrate was purified by flash column chromatography on silica gel with 2-10% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-e87267936b984c7fa59c899f95a2bffc
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07754886B2

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