Carbon tetrabromide → HCID 20032357, 화합물

HRID 231433노트

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HRID 231433 반응식
[Cl:1][C:2]1[C:7]([CH2:8]O)=[CH:6][C:5]([N:10]2[C:14](=[O:15])[C:13]3[CH2:16][CH2:17][CH2:18][CH2:19][C:12]=3[C:11]2=[O:20])=[C:4]([F:21])[CH:3]=1.C(Br)(Br)(Br)[Br:23].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(OCC)C>[Cl:1][C:2]1[C:7]([CH2:8][Br:23])=[CH:6][C:5]([N:10]2[C:14](=[O:15])[C:13]3[CH2:16][CH2:17][CH2:18][CH2:19][C:12]=3[C:11]2=[O:20])=[C:4]([F:21])[CH:3]=1

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 13629754N-(4-chloro-2-fluoro-5-hydroxymethylphenyl)-3,4,5,6-tetrahydrophthalimide

생성물 1

HCID 20032357HCID 20032357, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a stirred solution of 3.0 g (0.0097 mole) of of N-(4-chloro-2-fluoro-5-hydroxymethylphenyl)-3,4,5,6-tetrahydrophthalimide, prepared by the method of Example 4, and 6.4 g (0.0194 mole) of carbon tetrabromide in 30 ml of diethyl ether was added portionwise 5.1 g (0.0194 mole) of triphenylphosphine. This mixture was stirred overnight and was then filtered to remove the solid which had formed, and the solvent was evaporated under reduced pressure. The residue was passed through a column of silica gel. Appropriate fractions were combined, and the solvent was evaporated yielding 1.1 g of N-(4-chloro-2-fluoro-5-bromomethylphenyl)-3,4,5,6tetrahydrophthalimide as a white solid, m .p. 126°-128° C. The nmr and ir spectra were consistent with the proposed structure.

후처리

  1. filtrationwas then filtered
  2. customto remove the solid which
  3. customhad formed
  4. customthe solvent was evaporated under reduced pressure
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-aa65f84364d04a1e9bce2fd31f1bed1a
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04846882

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