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

HRID 1439292ノート

反応式

HRID 1439292 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-af604fec45c54c5095652e5a80610820
出典データセット
uspto-grants-1977_11
特許番号
US04058550

反応ノート

読み込み中…