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Hydrochloric Acid → trityloxy-acetic Acid Ethyl Ester

HRID 1714491
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HRID 1714491 반응식
[C:1](Cl)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:21]([O:25][CH2:26][CH3:27])(=[O:24])[CH2:22][OH:23].N1C=CC=CC=1.Cl>C(Cl)CCl>[CH2:26]([O:25][C:21](=[O:24])[CH2:22][O:23][C:1]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH3:27]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6456Trityl chlorideHCID 12184Ethyl Glycolate

생성물 1

HCID 12230788trityloxy-acetic Acid Ethyl Ester

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
40 °C

실험 절차

Trityl chloride (279 g, 1.0 mol) was dissolved in EDC (680 ml, 5 ml/g with respect to ethyl glycolate), and ethyl glycolate (135 g, 1.3 mol) was added to the mixture. Pyridine (99 g, 1.25 mol) was added thereto, and the mixture was stirred for 19 hours at 40° C. After completion of the reaction was confirmed by HPLC, 0.5 N aqueous hydrochloric acid solution (270 ml, 2 ml/g with respect to ethyl glycolate) was added to make the reaction solution a two-phase solution, which was then extracted. After the extraction was performed once again, EDC was distilled under reduced pressure. In order to obtain the compound of formula (8) as a solid form, hexane (680 ml) was added to the concentrated compound, the temperature was lowered to 0° C., and the mixture was stirred for about 3 hours and filtered.

후처리

  1. additionwas added
  2. extractionwas then extracted
  3. extractionAfter the extraction
  4. distillationEDC was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-9f0efe9728874fb78787a3eea89ecbbb
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07795463B2

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