Bis-Aminoethylglycol → HCID 67367938、化合物

HRID 625147

反応式

HRID 625147 の反応式
[CH3:1][C@@H:2]([C@@H:9]1[C@@:13]2([CH3:31])[CH2:14][CH2:15][CH:16]3[C@@:21]4([CH3:30])[CH2:22][CH2:23][CH:24]([O:26][C:27](Cl)=[O:28])[CH2:25][C:20]4=[CH:19][CH2:18][CH:17]3[CH:12]2[CH2:11][CH2:10]1)[CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7].[CH2:32]([CH2:37][O:38][CH2:39][CH2:40][NH2:41])[O:33][CH2:34][CH2:35][NH2:36]>ClCCl>[CH3:1][C@@H:2]([C@@H:9]1[C@:13]2([CH3:31])[C@H:12]([C@H:17]3[C@H:16]([CH2:15][CH2:14]2)[C@:21]2([CH3:30])[C:20]([CH2:25][C@@H:24]([O:26][C:27](=[O:28])[NH:36][CH2:35][CH2:34][O:33][CH2:32][CH2:37][O:38][CH2:39][CH2:40][NH2:41])[CH2:23][CH2:22]2)=[CH:19][CH2:18]3)[CH2:11][CH2:10]1)[CH2:3][CH2:4][CH2:5][CH:6]([CH3:8])[CH3:7]

参加物

4

反応物 2

HCID 70248Bis-AminoethylglycolHCID 54236888C28H45ClO2

生成物 1

HCID 67367938HCID 67367938、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

A solution of cholesteryl chloroformate (1 g, 2.23 mmol) in 25 mL dichloromethane was added dropwise under stirring to a solution of 2,2′-(ethylenedioxy)bis-(ethylamine) (495 mg, 3.34 mmol) in 75 mL dichloromethane. The reaction was stirred overnight at room temperature. The reaction was diluted with dichloromethane and extracted with water. The organic extract was dried over anhydrous MgSO4 dihydrate, filtered and evaporated. After purification on amino-modified silica gel (eluent: MeCl2→MeCl2/MeOH=975:25 v/v) the product (615 mg) was obtained as a white, waxy solid. MS (ISP): (M+H) 561.5

後処理

  1. extractionextracted with water
  2. extractionThe organic extract
  3. dry with materialwas dried over anhydrous MgSO4 dihydrate
  4. filtrationfiltered
  5. customevaporated
  6. customAfter purification on amino-modified silica gel (eluent: MeCl2→MeCl2/MeOH=975:25 v/v) the product (615 mg)
  7. customwas obtained as a white, waxy solid

出典と根拠

ORDレコード
ord-e5566a34280a453092c899a8032a84aa
出典データセット
uspto-grants-2016_04
特許番号
US09301990B2

関連ノート

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