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Sulfuric Acid → HCID 14698589、化合物

HRID 846212
ノート
印刷プレビュー

反応式

HRID 846212 の反応式
[CH3:1][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][C:20](OCC)=[O:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:4])[CH3:3].[H-].[Al+3].[Li+].[H-].[H-].[H-].C(OCC)C.S(=O)(=O)(O)O>O>[CH3:4][C:2]([C:5]1[CH:26]=[CH:25][C:8]([C:9]([NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][CH2:19][CH2:20][OH:21])=[CH:14][CH:13]=2)=[O:10])=[CH:7][CH:6]=1)([CH3:1])[CH3:3]
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 4

HCID 1118Sulfuric AcidHCID 3283Diethyl EtherHCID 14698592HCID 14698592、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 14698589HCID 14698589、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2.2 g. of the compound of Example 31 are reduced with 0.65 g. lithium aluminum hydride in 50 ml. boiling diethyl ether. The reaction mixture is mixed with water, sufficient 10% sulphuric acid is added thereto just to dissolve the precipitate, extracted with diethyl ether, evaporated to dryness and the remaining oil purified by column chromatography (silica gel; dichloromethane/methanol 99:1 v/v). The appropriate fractions are evaporated to dryness in a vacuum, the residue is first recrystallised from ethyl acetate/ligroin (1:1 v/v) and then from toluene to give 0.6 g. (31% of theory) of the title compound; m.p. 136°-142° C.

後処理

  1. additionis added
  2. dissolutionjust to dissolve the precipitate
  3. extractionextracted with diethyl ether
  4. customevaporated to dryness
  5. customthe remaining oil purified by column chromatography (silica gel; dichloromethane/methanol 99:1 v/v)
  6. customThe appropriate fractions are evaporated to dryness in a vacuum
  7. customthe residue is first recrystallised from ethyl acetate/ligroin (1:1 v/v)
  8. customfrom toluene to give 0.6 g

出典と根拠

ORDレコード
ord-098980a05fcb4283b1431d7bc71a6412
出典データセット
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05135949

反応ノート

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