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Carbon tetrabromide → HCID 18331400, 화합물

HRID 2270558
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HRID 2270558 반응식
[CH2:1]([O:3][C:4]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6]O)[CH3:2].C(Br)(Br)(Br)[Br:16].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[CH2:1]([O:3][C:4]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6][Br:16])[CH3:2]
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참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 86201264HCID 86201264, 화합물

생성물 1

HCID 18331400HCID 18331400, 화합물수율 87%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a mixture of the compound (3.13 g) obtained in Example 417b, carbon tetrabromide (5.26 g) and methylene chloride (100 ml), triphenylphosphine (4.16 g) was added under ice cooling. The reaction mixture was stirred under ice cooling for 30 min and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate: n-hexane=1:9) to give 3.59 g of the titled compound (yield, 87%).

후처리

  1. additionwas added under ice cooling
  2. concentrationconcentrated under reduced pressure
  3. customThe resulting residue was purified by silica gel column chromatography (eluent, ethyl acetate: n-hexane=1:9)

출처 및 근거

ORD 기록
ord-b2416b45a35548c5bfc7da59f79fa1fd
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06331553B1

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