ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Formaldehyde → 2-Butyl-2-ethyl-1,3-propanediol

HRID 53411
ノート
印刷プレビュー

反応式

HRID 53411 の反応式
[CH2:1]([CH:3]([CH2:6][CH2:7][CH2:8][CH3:9])[CH:4]=[O:5])[CH3:2].C=O.C([C:14](=[O:20])CCCCC)C.S(=O)(=O)(O)O>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-]>[CH2:6]([C:3]([CH2:1][CH3:2])([CH2:14][OH:20])[CH2:4][OH:5])[CH2:7][CH2:8][CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 712Formaldehyde4 回HCID 1118Sulfuric AcidHCID 312412-Ethylhexanal2 回HCID 2467283-Octanone

生成物 1

HCID 610382-Butyl-2-ethyl-1,3-propanediol

試薬・触媒・溶媒 2

HCID 21218Trioctylmethylammonium chloride触媒
HCID 94433
Tetrabutylammonium hydrogen sulfate
触媒

実験手順

The molar ratio of the 2-ethyl hexanal to the formaldehyde, used as the initial materials of the reaction, should be within the range 1:2 to 1:4, preferably within the range 1:2.5 to 1:3.5. To the mixture is added a neutral or cationic phase transfer catalyst, such as neutral polyethylene glycol (e.g. PEG 400) or a cationic tetrabutylammoniumhydrogen sulfate (TBAHSO4) or tricaprylmethylammonium chloride (Aliquat 336). These are added in an amount of 1-50% by weight, preferably 5-30% by weight, of the mass of the formalin solution or, if solid paraformaldehyde is used, in an amount of 1-20% by weight, preferably 3-10% by weight, of the mass of the aqueous solution and solid paraformaidehyde, or in an amount of 1-50% by weight, preferably 5-15% by weight, of the amount of 2-ethyl hexanal. The mixture of the initial materials is heated to 30°-100° C., preferably to 50°-80° C., and most preferably to 60°-80° C., and an aqueous solution of the alkali metal hydroxide or earth alkali metal hydroxide is added to the mixture, drop by drop, in the course of up to 5 h, preferably 1-3 h, and the reaction is continued at the said temperature for up to 3 h, preferably 15 min-2 h, most preferably 15 min-1 h 15 min. The alkali metal hydroxide or earth alkali metal hydroxide is used in a molar amount 1:1 to 2:1, preferably in a molar amount of 1.25:1 to 1.75:1 to that of 2:1-ethyl hexanal. After this reaction step the mixture is neutralized with an organic acid or a mineral acid, preferably for example sulfuric acid, and the phases are separated from each other, preferably while they are hot. The organic phase is washed with water once or several times, preferably 1-2 times, by using for the wash an amount of water at minimum 50% of the mass of the organic phase. The phases are separated and the organic phases are combined and vacuum distilled. The boiling point of the final product is 130°-132° C./9 mmHg. The yield obtained for 2-n-butyl-2-ethyl-1,3-propane diol was up to more than 92%, depending on the reaction conditions and the molar proportions.

後処理

  1. additionTo the mixture is added a neutral or cationic phase transfer catalyst
  2. temperatureis heated to 30°-100° C., preferably to 50°-80° C.
  3. custompreferably 1-3 h
  4. customup to 3 h
  5. custompreferably 15 min-2 h, most preferably 15 min-1 h 15 min
  6. customAfter this reaction step the mixture
  7. washThe organic phase is washed with water once
  8. washwash an amount of water at minimum 50% of the mass of the organic phase
  9. customThe phases are separated
  10. distillationvacuum distilled
  11. customis 130°-132° C.

出典と根拠

ORDレコード
ord-0a3b12ba229f46b59d238f05947e5219
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05618985

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート