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Hydrochloric Acid → trityloxy-acetic Acid Ethyl Ester

HRID 1776552
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HRID 1776552 반응식
Cl[C:2]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24].Cl>C(Cl)Cl>[C:2]([O:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6456Trityl chlorideHCID 12184Ethyl Glycolate

생성물 1

HCID 12230788trityloxy-acetic Acid Ethyl Ester수율 67.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
50 °C

실험 절차

To a solution of (chloromethanetriyl)tribenzene (9.8 g, 35.2 mmol) in DCM (500 ml), ethyl 2-hydroxyacetate (4.33 ml, 45.7 mmol) and Py (3.70 ml, 45.7 mmol) were added at RT. The reaction was heated at 50° C. for 9 hours. HCl 2N was added to the mixture, and the organic phase was separated, dried over Na2SO4 and evaporated under vacuum. The resulting white solid was triturated in Hexane. Ethyl 2-(trityloxy)acetate was obtained (8.2 g, 23.67 mmol, 67.3% yield) and used in the following step without further purification.

후처리

  1. customthe organic phase was separated
  2. dry with materialdried over Na2SO4
  3. customevaporated under vacuum
  4. customThe resulting white solid was triturated in Hexane

출처 및 근거

ORD 기록
ord-e07fa50800ff44a796b3236562ab945d
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09265768B2

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