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Hydrochloric Acid → HCID 20489855, 화합물

HRID 1447643
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HRID 1447643 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6](Cl)=[O:7].C1(C2[NH:24][CH2:23][CH:22]([CH2:25][Cl:26])[O:21]2)C=CC=CC=1.Cl>C(Cl)(Cl)Cl.N1C=CC=CC=1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6]([NH:24][CH2:23][CH:22]([OH:21])[CH2:25][Cl:26])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 77070Veratroyl chlorideHCID 2707015-(Chloromethyl)-2-phenyl-1,3-oxazolidine

생성물 1

HCID 20489855HCID 20489855, 화합물수율 72.3%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6212Chloroform용매2회

실험 절차

At a temperature of -40° C., a solution of 15.2 g 3,4-dimethoxybenzoyl chloride in 40 ml of chloroform is added dropwise to a solution of 15.0 g of 2-phenyl-5-chloromethyloxazolidine in a mixture of 200 ml of chloroform and 6 ml of pyridine. The mixture is heated to room temperature. After a reaction period of 14 hours, 20 ml of concentrated hydrochloric acid are added, the phases are thoroughly mixed for 10 minutes, and then separated. The separated aqueous phase is diluted with water to twice its volume and is saturated with sodium chloride. Then it is extracted with chloroform. After drying the chloroform extract and evaporating the solvent, 15.0 g of N-(3,4-dimethoxybenzoyl)-3-chloro-1-aminopropan-2-ol is obtained as an oil which can be used in the following reaction without any prior purification. After crystallization from ethanol/toluene, the compound melts at 104°-106° C.

후처리

  1. additionare added
  2. additionthe phases are thoroughly mixed for 10 minutes
  3. customseparated
  4. additionThe separated aqueous phase is diluted with water to twice its volume
  5. extractionThen it is extracted with chloroform
  6. dry with materialAfter drying the chloroform
  7. extractionextract
  8. customevaporating the solvent

출처 및 근거

ORD 기록
ord-b064941fb30345fd899bfcbda2f683e0
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04177287

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