Triethylamine → HCID 17910428, 화합물

HRID 2187728노트

반응식

HRID 2187728 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 17910428HCID 17910428, 화합물수율 90.8%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-470ff53f36254e118014353406276740
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06410581B1

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