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Oxalyl chloride → HCID 13281349, 화합물

HRID 2164838
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HRID 2164838 반응식
[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
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참가 물질

4

반응물 2

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

생성물 1

HCID 13281349HCID 13281349, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2e7a9bfc10f74ec4b684c42ed16fbaf9
출처 데이터셋
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04507317

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