3-Chloro-1,2-propanediol → 1,2-Dihydroxypropane dodecyl sulfide

HRID 1153699

反応式

HRID 1153699 の反応式
[OH-].[Na+].[CH2:3]([SH:15])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].Cl[CH2:17][CH:18]([OH:21])[CH2:19][OH:20]>C(O)(C)C>[CH2:3]([S:15][CH2:17][CH2:18][CH2:19][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11])[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].[OH:20][CH2:19][CH:18]([OH:21])[CH3:17]

参加物

5

反応物 3

HCID 72903-Chloro-1,2-propanediolHCID 81951-DodecanethiolHCID 14798Sodium Hydroxide

生成物 1

HCID 867397751,2-Dihydroxypropane dodecyl sulfide

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
80 °C

実験手順

Approximately 397 g of 50% aqueous sodium hydroxide solution was added dropwise over a period of 7 hours to a solution of n-dodecyl mercaptan (1000g) and 1-chloropropane-2,3-diol (547g) in isopropanol solvent (2000 cc) at ambient temperature. The reaction temperature rose from 21° to 56° C. during the addition. The reaction was refluxed for 5 hours at 80° C. and then filtered hot through paper to remove the precipitated salt. The isopropanol solvent was removed by distillation. The product residue was dissolved in about 4000 cc of toluene and washed with water several times. The toluene solution was dried over magnesium sulfate and filtered through diatomaceous earth. Toluene was removed by high speed rotary evaporation to yield a white solid product.

後処理

  1. additionThe reaction temperature rose from 21° to 56° C. during the addition
  2. filtrationfiltered hot through paper
  3. customto remove the precipitated salt
  4. customThe isopropanol solvent was removed by distillation
  5. dissolutionThe product residue was dissolved in about 4000 cc of toluene
  6. washwashed with water several times
  7. dry with materialThe toluene solution was dried over magnesium sulfate
  8. filtrationfiltered through diatomaceous earth
  9. customToluene was removed by high speed rotary evaporation
  10. customto yield a white solid product

出典と根拠

ORDレコード
ord-969c057dd3d9439fa55ffda69fe69457
出典データセット
uspto-grants-1984_12
特許番号
US04486323

関連ノート

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