Hydrochloric Acid → 1-Decyn-4-ol

HRID 256735ノート

反応式

HRID 256735 の反応式
Cl[C:2](=[CH2:12])[CH2:3][CH:4]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])[OH:5].[OH-].[Na+].Cl>CN(C)C=O>[CH2:6]([CH:4]([CH2:3][C:2]#[CH:12])[OH:5])[CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11030613HCID 11030613、化合物

生成物 1

HCID 5441861-Decyn-4-ol収率 97%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

20.00 Grams of the 2-chloroallyl-n-hexylcarbinol obtained above were dissolved in 200 g of N,N-dimethylformamide, and 8.39 g of sodium hydroxide in a flake form were added. The resultant mixture was stirred at 25° C. for 10 hours. After the reaction was completed the reaction mixture was neutralized with concentrated hydrochloric acid, and insolubles were filtered off. After the filtrate was concentrated under reduced pressure, the concentration residue was subjected to extraction with toluene, washed with a 7% sodium carbonate aqueous solution and then dried over sodium sulfate. The desiccant was filtered off, and the toluene was distilled off. The resultant oily substance was distilled under reduced pressure to give 15.70 g of n-hexylpropargylcarbinol. The results were as follows.

後処理

  1. filtrationwere filtered off
  2. concentrationAfter the filtrate was concentrated under reduced pressure
  3. extractionthe concentration residue was subjected to extraction with toluene
  4. washwashed with a 7% sodium carbonate aqueous solution
  5. dry with materialdried over sodium sulfate
  6. filtrationThe desiccant was filtered off
  7. distillationthe toluene was distilled off
  8. distillationThe resultant oily substance was distilled under reduced pressure

出典と根拠

ORDレコード
ord-2d95b47f0c38412a96f6c67693b06f61
出典データセット
uspto-grants-1993_11
特許番号
US05258529

反応ノート

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