Epichlorohydrin → HCID 23113189、化合物

HRID 2355800ノート

反応式

HRID 2355800 の反応式
[O:1]1[CH2:5][CH2:4][CH2:3]C1.[OH:6][CH2:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][C:10]([CH2:18][OH:19])([CH2:11]3)[CH2:9]1)[CH2:15]2.[H-].[Na+].[CH2:22]([CH:24]1[O:26][CH2:25]1)Cl>C(Cl)(Cl)Cl>[CH2:22]([O:6][CH2:7][C:8]12[CH2:15][CH:14]3[CH2:13][CH:12]([CH2:11][C:10]([CH2:18][O:19][CH2:3][CH:4]4[O:1][CH2:5]4)([CH2:16]3)[CH2:9]1)[CH2:17]2)[CH:24]1[O:26][CH2:25]1

参加物

6

反応物 4

HCID 7835EpichlorohydrinHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 7030111,3-Adamantanedimethanol

生成物 1

HCID 23113189HCID 23113189、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

300 ml of dehydrated tetrahydrofuran containing 19.6 g (0.1 mol) of 1,3-bis(hydroxymethyl)adamantane and 5.3 g (0.22 mol) of sodium hydride was stirred in a nitrogen atmosphere at the reflux temperature for 2 hours. Thereto was dropwise added 20.4 g (0.22 mol) of epichlorohydrin, followed by stirring at the reflux temperature for 12 hours. To the reaction mixture was added 200 ml of chloroform, followed by washing with water. The chloroform layer was dried with magnesium sulfate. The dried chloroform layer was subjected to distillation under reduced pressure for solvent removal, whereby was obtained a white solid and oily matter.

後処理

  1. washby washing with water
  2. dry with materialThe chloroform layer was dried with magnesium sulfate
  3. distillationThe dried chloroform layer was subjected to distillation under reduced pressure for solvent removal
  4. customwhereby was obtained a white solid and oily matter

出典と根拠

ORDレコード
ord-5772540f082e4804b2a7718f9593e7bf
出典データセット
uspto-grants-2010_07
特許番号
US07754903B2

反応ノート

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