Triethylamine → HCID 17910428、化合物

HRID 2187728ノート

反応式

HRID 2187728 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH:5]=[C:6]([Cl:9])[C:7]=1[OH:8].C(N(CC)CC)C.Cl[C:24]([O:26][CH2:27][CH3:28])=[O:25]>C(OCC)(=O)C>[C:24](=[O:25])([O:26][CH2:27][CH3:28])[O:8][C:7]1[C:2]([Cl:1])=[CH:3][C:4]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:5][C:6]=1[Cl:9]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 708204-Hydroxy-3,5-dichlorobiphenyl

生成物 1

HCID 17910428HCID 17910428、化合物収率 90.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

40.6 g (0.17 mol) of 3,5-dichloro-4-hydroxybiphenyl (prepared according to J. C. Colbert et al., JACS 56, 202 (1934)) and 17.2 g (0.17 mol) of triethylamine are dissolved in 170 ml of ethyl acetate and admixed dropwise with 18.4 g (0.17 mol) of ethyl chloroformate at 10° C. The reaction solution is stirred overnight and washed with water, and the organic phase is concentrated. For further purification, the crude product (51.2 g) is chromatographed over silica gel using the system chloroform. 48 g (yield 90.8% of theory) of (2,6-dichloro-4-phenyl-phenyl) ethyl carbonate are obtained as an oil, log p (pH 7.5): 4.65.

後処理

  1. washwashed with water
  2. concentrationthe organic phase is concentrated
  3. customFor further purification
  4. customthe crude product (51.2 g) is chromatographed over silica gel using the system chloroform

出典と根拠

ORDレコード
ord-470ff53f36254e118014353406276740
出典データセット
uspto-grants-2002_06
特許番号
US06410581B1

反応ノート

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