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Hydrochloric Acid → HCID 20489855、化合物

HRID 1701180
ノート
印刷プレビュー

反応式

HRID 1701180 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 temperature 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-63524c6d042b45f0a959b571a658f3e8
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04191770

反応ノート

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