Carbon tetrabromide → HCID 20032357、化合物

HRID 231433ノート

反応式

HRID 231433 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 20032357HCID 20032357、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aa65f84364d04a1e9bce2fd31f1bed1a
出典データセット
uspto-grants-1989_07
特許番号
US04846882

反応ノート

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