Hydrochloric Acid → HCID 86748043、化合物

HRID 1741635ノート

反応式

HRID 1741635 の反応式
[OH:1][CH:2]([CH2:21][N:22]([C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])[CH2:23][CH2:24][CH3:25])[CH2:3][O:4][CH:5]([CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:7].[H-].[Na+].S(OC)(O[CH3:39])(=O)=O.Cl>CN(C=O)C>[CH3:39][O:1][CH:2]([CH2:21][N:22]([C:26]([O:28][C:29]([CH3:31])([CH3:30])[CH3:32])=[O:27])[CH2:23][CH2:24][CH3:25])[CH2:3][O:4][CH:5]([CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:7]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 24758Sodium hydrideHCID 86748044HCID 86748044、化合物

生成物 1

HCID 86748043HCID 86748043、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

5 g. (11.3 mMol) 2-[2-hydroxy-3-(tert.-butyloxycarbonyl-propylamino)-propoxy]-3-phenyl-propiophenone are dissolved in 50 ml. abs. DMF and mixed at 0° C. with 0.30 g. (12.5 mMol) sodium hydride. Thereafter, it is stirred for 70 minutes at room temperature. Subsequently, the reaction mixture is cooled to 0° C. and a solution of 1.60 g. (12.5 mMol) dimethyl sulphate in 5 ml. absolute DMF added dropwise thereto. After 40 minutes at 0° to 5° C., the reaction mixture is emptied into 2N HCl. The phases are separated and the H2O phase extracted three times with CH2Cl2. The combined organic phases are after drying over Na2SO4, evaporated. There are obtained 4.5 g. of an orange oil which is purified column chromatographically. Column chromatography: silica gel, Bz:EE=14:1. The purified oil crystallises in a low-cooling cabinet.

後処理

  1. temperatureSubsequently, the reaction mixture is cooled to 0° C.
  2. waitAfter 40 minutes at 0° to 5° C.
  3. customThe phases are separated
  4. extractionthe H2O phase extracted three times with CH2Cl2
  5. dry with materialafter drying over Na2SO4
  6. customevaporated
  7. customThere are obtained 4.5 g
  8. customof an orange oil which is purified column chromatographically
  9. customThe purified oil crystallises in a low-cooling cabinet

出典と根拠

ORDレコード
ord-c1413b33497f4fc2802b3a4331e8e64d
出典データセット
uspto-grants-1994_08
特許番号
US05334602

反応ノート

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