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Oxalyl chloride → HCID 13281349、化合物

HRID 544684
ノート
印刷プレビュー

反応式

HRID 544684 の反応式
[Cl:1][C:2]1[C:3]([CH2:14][CH2:15][CH2:16][C:17]([OH:19])=O)=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.C(Cl)(=O)C([Cl:23])=O>C1(C)C=CC=CC=1>[Cl:1][C:2]1[C:3]([CH2:14][CH2:15][CH2:16][C:17]([Cl:23])=[O:19])=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 65578Oxalyl chlorideHCID 132813484-(3-Chloro[1,1'-biphenyl]-2-yl)butanoic acid

生成物 1

HCID 13281349HCID 13281349、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Under a dry argon atmosphere a stirred solution of 4-(3-chloro[1,1'-biphenyl]-2-yl)butanoic acid (22.8 g, 0.083 mole) in toluene (500 ml) was heated at 65°. Oxalyl chloride (21 g, 0.166 mole) was added slowly to the reaction mixture. After complete addition the mixture was allowed to stir at 40° for approximately 18 hours. The solvent and excess oxalyl chloride were removed by distillation under reduced pressure. Further distillation under reduced pressure gave 4-(3-chloro[1,1'-biphenyl]-2-yl)butanoic acid chloride (b.p. 150°/0.04 mm) as a clear oil. The nmr spectrum was consistent with the proposed structure.

後処理

  1. additionAfter complete addition the mixture
  2. customThe solvent and excess oxalyl chloride were removed by distillation under reduced pressure
  3. distillationFurther distillation under reduced pressure

出典と根拠

ORDレコード
ord-cd01fcaf743d43ab80cce1740bf0ecfc
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04451484

反応ノート

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