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3-Tert-butylamino-1,2-propanediol → HCID 21388032、化合物

HRID 1833878
ノート
印刷プレビュー

反応式

HRID 1833878 の反応式
[K].[C:2]([NH:6][CH2:7][CH:8]([OH:11])[CH2:9][OH:10])([CH3:5])([CH3:4])[CH3:3].Cl[C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([Cl:23])[CH:21]=2)[C:16]([CH3:24])=[CH:15][N:14]=1>C(O)(C)(C)C>[OH:11][CH:8]([CH2:7][NH:6][C:2]([CH3:5])([CH3:4])[CH3:3])[CH2:9][O:10][C:13]1[C:22]2[C:17](=[CH:18][CH:19]=[C:20]([Cl:23])[CH:21]=2)[C:16]([CH3:24])=[CH:15][N:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 908313-Tert-butylamino-1,2-propanediolHCID 5462222PotassiumHCID 21388031HCID 21388031、化合物

生成物 1

HCID 21388032HCID 21388032、化合物

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒

実験手順

0.74 g of Potassium is dissolved in 40 ml of tert.-butylalcohol and 3.0 g of 1-tert.butylamino-2,3-dihydroxypropane and subsequently 4 g of 1,7-dichloro-4-methylisoquinoline are added. After stirring for one day, heating up to 50° is effected for a further day. The reaction solution is concentrated by evaporation under vacuum. The residue is taken up with 1N hydrochloric acid and ether, the aqueous phase neutralised with 2N caustic soda solution and extracted with methylene chloride. After drying over magnesium sulphate and concentration by evaporation the title compound is obtained in free base form. M.p. 116°-117°.

後処理

  1. temperatureheating up to 50°
  2. waitis effected for a further day
  3. concentrationThe reaction solution is concentrated by evaporation under vacuum
  4. extractionextracted with methylene chloride
  5. dry with materialAfter drying over magnesium sulphate and concentration by evaporation the title compound
  6. customis obtained in free base form

出典と根拠

ORDレコード
ord-e2f5d66b05ea481b859468b98d6716fa
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04067873

反応ノート

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