1-[N-[2-(3-carbamoyl-4-hydroxyphenoxy)ethyl]-benzylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanol → 1-[2-(3-Carbamoyl-4-hydroxyphenoxy)ethylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanol

HRID 4556노트

반응식

HRID 4556 반응식
[C:1]([C:4]1[CH:5]=[C:6]([CH:33]=[CH:34][C:35]=1[OH:36])[O:7][CH2:8][CH2:9][N:10](CC1C=CC=CC=1)[CH2:11][CH:12]([OH:25])[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][OH:24])=[CH:17][CH:16]=1)(=[O:3])[NH2:2].[H][H]>CO.[Pd]>[C:1]([C:4]1[CH:5]=[C:6]([CH:33]=[CH:34][C:35]=1[OH:36])[O:7][CH2:8][CH2:9][NH:10][CH2:11][CH:12]([OH:25])[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH2:22][CH2:23][OH:24])=[CH:17][CH:16]=1)(=[O:3])[NH2:2]

참가 물질

5

반응물 2

HCID 201513021-[N-[2-(3-carbamoyl-4-hydroxyphenoxy)ethyl]-benzylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanolHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 201513041-[2-(3-Carbamoyl-4-hydroxyphenoxy)ethylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanol

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A solution of 23 g of crude 1-[N-[2-(3-carbamoyl-4-hydroxyphenoxy)ethyl]-benzylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanol in 500 ml of methanol is hydrogenated, under normal conditions, with the addition of 2 g of 5% palladium on carbon catalyst, until hydrogen absorption has ceased. The catalyst is then removed by filtration and the filtrate is concentrated by evaporation under reduced pressure. The crystalline residue is stirred in a mixture of 50 ml of methanol and ether. The crystals so obtained are isolated by filtration and dried in vacuo, affording 1-[2-(3-carbamoyl-4-hydroxyphenoxy)ethylamino]-3-[4-(2-hydroxyethoxy)phenoxy]-2-propanol with a melting point of 150°-151° C. Reaction with the equivalent amount of hydrogen chloride, as solution in methanol, affords the hydrochloride with a melting point of 205°-206° C.

후처리

  1. customThe catalyst is then removed by filtration
  2. concentrationthe filtrate is concentrated by evaporation under reduced pressure
  3. customThe crystals so obtained
  4. customare isolated by filtration
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-a3fc75976eb84e38ac08b331292e5971
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727067

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