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

HRID 615050노트

반응식

HRID 615050 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d2a37d301d0f45c3b32c942264c3db39
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04146546

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