홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1-Hydroxybenzotriazole → HCID 66864043, 화합물

HRID 2093430
노트
인쇄 미리보기

반응식

HRID 2093430 반응식
ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[Cl:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([C:49]2[CH:54]=[CH:53][C:52]([Cl:55])=[CH:51][CH:50]=2)[N:31]2[CH2:34][CH:33]([CH2:35][S:36]([NH:39][C:40]3[CH:41]=[C:42]([CH:46]=[CH:47][CH:48]=3)[C:43]([OH:45])=O)(=[O:38])=[O:37])[CH2:32]2)=[CH:26][CH:25]=1.Cl.[NH2:57][CH2:58][C:59]([N:61]1[CH2:66][CH2:65][O:64][CH2:63][CH2:62]1)=[O:60]>O1CCCC1.ClCCl.C(N(CC)CC)C>[Cl:23][C:24]1[CH:25]=[CH:26][C:27]([CH:30]([C:49]2[CH:54]=[CH:53][C:52]([Cl:55])=[CH:51][CH:50]=2)[N:31]2[CH2:34][CH:33]([CH2:35][S:36]([NH:39][C:40]3[CH:41]=[C:42]([CH:46]=[CH:47][CH:48]=3)[C:43]([NH:57][CH2:58][C:59]([N:61]3[CH2:66][CH2:65][O:64][CH2:63][CH2:62]3)=[O:60])=[O:45])(=[O:37])=[O:38])[CH2:32]2)=[CH:28][CH:29]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 122918142-Amino-1-(morpholin-4-yl)ethan-1-one--hydrogen chloride (1/1)HCID 66864534HCID 66864534, 화합물

생성물 1

HCID 66864043HCID 66864043, 화합물

시약·촉매·용매 3

HCID 6344
Dichloromethane
용매
HCID 8028Tetrahydrofuran용매
HCID 8471Triethylamine용매

반응 조건

온도
20 °C

실험 절차

67 mg of 1-hydroxybenzotriazole, 0.14 cm3 of triethylamine and 270 mg of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride are added successively to a solution of 500 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)benzoic acid and 215 mg of 2-amino-1-morpholin-4-ylethanone hydrochloride in 15 cm3 of tetrahydrofuran. The reaction mixture is left stirring overnight at a temperature in the region of 20° C. After concentration of the reaction medium to dryness under reduced pressure, the residue obtained is taken up with dichloromethane. The organic phase is washed with water, dried, and concentrated to dryness under reduced pressure, to give a reaction crude which is purified by flash chromatography on a Merck 30 g silica cartridge (elution gradient: 100/0 to 95/5 dichloromethane/methanol). After concentration of the fractions under reduced pressure, a white foam is obtained which crystallizes after trituration with diethyl ether. After filtration and drying using a vane pump, 470 mg of 3-({1-[bis(4-chlorophenyl)methyl]azetidin-3-yl}methanesulphonylamino)-N-(2-morpholin-4-yl-2-oxoethyl)benzamide are thus obtained in the form of white crystals.

후처리

  1. waitThe reaction mixture is left
  2. customAfter concentration of the reaction medium to dryness under reduced pressure, the residue obtained
  3. washThe organic phase is washed with water
  4. customdried
  5. concentrationconcentrated to dryness under reduced pressure
  6. customto give
  7. customa reaction crude which
  8. customis purified by flash chromatography on a Merck 30 g silica cartridge (elution gradient: 100/0 to 95/5 dichloromethane/methanol)
  9. customAfter concentration of the fractions under reduced pressure, a white foam is obtained which
  10. customcrystallizes after trituration with diethyl ether
  11. filtrationAfter filtration
  12. customdrying
  13. customare thus obtained in the form of white crystals

출처 및 근거

ORD 기록
ord-9b24d917cc614ef9928ca4e68d8cf6f7
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08445478B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트