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Hydrochloric Acid → HCID 20489855、化合物

HRID 1995187
ノート
印刷プレビュー

反応式

HRID 1995187 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 20489855HCID 20489855、化合物収率 72.3%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 6212Chloroform溶媒2 回

実験手順

A solution of 15.2 g of 3,4-dimethoxybenzoyl chloride in 40 ml of chloroform is added dropwise to a solution of 15.0 g 2-phenyl-5-chloromethyloxazolidine in a mixture of 200 ml of chloroform and 6 ml of pyridine at a temperture of -40° C. under agitation. This solution is then 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 a period of 10 minutes and then are separated. The separated aqueous phase is diluted with water to twice its volume and then is saturated with sodium chloride and 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 further reacted without any purification. After crystallization from ethanol/toluene the compound exhibits a melting point of 104°-106° C.

後処理

  1. additionare added
  2. additionthe phases are thoroughly mixed for a period of 10 minutes
  3. customare separated
  4. additionThe separated aqueous phase is diluted with water to twice its volume
  5. extractionextracted with chloroform
  6. dry with materialAfter drying the chloroform-
  7. extractionextract
  8. customevaporating the solvent

出典と根拠

ORDレコード
ord-c0a5493d13834cb1b167c1cf30a93e98
出典データセット
uspto-grants-1983_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04402981

反応ノート

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