Water → Ethyl 4-({3-[4-(benzyloxy)phenyl]propyl}amino)benzoate

HRID 2052507노트

반응식

HRID 2052507 반응식
CS(O[CH2:6][CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][CH:10]=1)(=O)=O.CN(C)P(N(C)C)(N(C)C)=O.[NH2:34][C:35]1[CH:45]=[CH:44][C:38]([C:39]([O:41][CH2:42][CH3:43])=[O:40])=[CH:37][CH:36]=1.O>C(O)C>[CH2:16]([O:15][C:12]1[CH:13]=[CH:14][C:9]([CH2:8][CH2:7][CH2:6][NH:34][C:35]2[CH:36]=[CH:37][C:38]([C:39]([O:41][CH2:42][CH3:43])=[O:40])=[CH:44][CH:45]=2)=[CH:10][CH:11]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 2337BenzocaineHCID 12679HexamethylphosphoramideHCID 13079701HCID 13079701, 화합물

생성물 1

HCID 13079684Ethyl 4-({3-[4-(benzyloxy)phenyl]propyl}amino)benzoate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 12.8 g. of 3-[p-(benzyloxy)phenyl]propanol O-methanesulfonate (prepared as described in Example 43), 50 ml. of hexamethylphosphoramide and 16.5 g. of ethyl p-aminobenzoate is heated at 100°-105° C. for 17.5 hours. The mixture is chilled, diluted with 15 ml. of water, 30 ml. of ethanol and chilled. In order to filter, 100 ml. of ethanol-water (1:1) is added and the solid filtered and washed with ethanol-water (1:1) and with water to give tan crystals, m.p. 98°-107° C. Recrystallization from ethanol gives light tan crystals, m.p. 114°-116° C.

후처리

  1. additionA mixture of 12.8 g
  2. temperatureThe mixture is chilled
  3. additiondiluted with 15 ml
  4. filtrationIn order to filter
  5. additionof ethanol-water (1:1) is added
  6. filtrationthe solid filtered
  7. washwashed with ethanol-water (1:1) and with water
  8. customto give tan crystals, m.p. 98°-107° C
  9. customRecrystallization from ethanol
  10. customgives light tan crystals, m.p. 114°-116° C.

출처 및 근거

ORD 기록
ord-d23ae89ae02b4af8a67acc297f0cb53b
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04185115

반응 노트

불러오는 중…