Hexamethylphosphoramide → 4-Hydroxybutyl 4-(n-hexadecylamino)benzoate

HRID 615050ノート

反応式

HRID 615050 の反応式
[CH2:1]([NH:17][C:18]1[CH:26]=[CH:25][C:21]([C:22]([O-:24])=[O:23])=[CH:20][CH:19]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].[Na+].Cl[CH2:29][CH2:30][CH2:31][CH2:32][OH:33].CN(C)P(N(C)C)(N(C)C)=O>O>[CH2:1]([NH:17][C:18]1[CH:19]=[CH:20][C:21]([C:22]([O:24][CH2:29][CH2:30][CH2:31][CH2:32][OH:33])=[O:23])=[CH:25][CH:26]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 12679HexamethylphosphoramideHCID 135694-Chloro-1-butanolHCID 23703815Cetaben Sodium

生成物 1

HCID 130193784-Hydroxybutyl 4-(n-hexadecylamino)benzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

A mixture of 7.66 g of sodium 4-(n-hexadecylamino)benzoate, 7.55 g of 4-chloro-1-butanol, and 20.0 ml of hexamethylphosphoramide is stirred at 150° C. for two hours, allowed to cool, and poured into water. The solid is collected by filtration and then is dissolved in methylene chloride. The solution is washed with water, dried, and evaporated. The residual solid is crystallized from hexane to yield 4-hydroxybutyl 4-(n-hexadecylamino)benzoate as a white solid, mp 61°-63° C.

後処理

  1. temperatureto cool
  2. filtrationThe solid is collected by filtration
  3. dissolutionis dissolved in methylene chloride
  4. washThe solution is washed with water
  5. customdried
  6. customevaporated
  7. customThe residual solid is crystallized from hexane

出典と根拠

ORDレコード
ord-d2a37d301d0f45c3b32c942264c3db39
出典データセット
uspto-grants-1979_03
特許番号
US04146546

反応ノート

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