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

Triethylamine → 2-Butyl-benzofuran-3-carboxylic acid benzyl-(6-hydroxy-naphthalen-2-ylmethyl)-amide

HRID 1357295
노트
인쇄 미리보기

반응식

HRID 1357295 반응식
[CH2:1]([C:5]1[O:6][C:7]2[CH:16]=[CH:15][CH:14]=[CH:13][C:8]=2[C:9]=1[C:10](Cl)=[O:11])[CH2:2][CH2:3][CH3:4].[CH2:17]([NH:24][CH2:25][C:26]1[CH:27]=[C:28]2[C:33](=[CH:34][CH:35]=1)[CH:32]=[C:31]([OH:36])[CH:30]=[CH:29]2)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(N(CC)CC)C>C1COCC1.C(OCC)(=O)C>[CH2:17]([N:24]([CH2:25][C:26]1[CH:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[C:31]([OH:36])[CH:32]=2)[CH:27]=1)[C:10]([C:9]1[C:8]2[CH:13]=[CH:14][CH:15]=[CH:16][C:7]=2[O:6][C:5]=1[CH2:1][CH2:2][CH2:3][CH3:4])=[O:11])[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 185052776-(Benzylamino-methyl)-naphthalen-2-olHCID 185053462-Butyl-benzofuran-3-carbonyl chloride

생성물 1

HCID 691391852-Butyl-benzofuran-3-carboxylic acid benzyl-(6-hydroxy-naphthalen-2-ylmethyl)-amide수율 65.2%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회
HCID 8857
Ethyl Acetate
용매

실험 절차

2-Butyl-benzofuran-3-carbonyl-chloride (3 mmol), prepared in step 2 of Example 3, in 25 mL of anhydrous THF was added under nitrogen dropwise over 1 h to a solution of 6-(benzylamino-methyl)-naphthalen-2-ol (0.71 g, 2.7 mmol), prepared in the previous step, and triethylamine (0.376 mL, 2.7 mmol) in 75 mL of anhydrous THF at room temperature. After the addition the reaction was stirred at room temperature for 20 h (overnight). The solid present was removed by filtration and the filtrate concentrated under reduced pressure to give a brown oil. The oil was dissolved in ethyl acetate and extracted with 1N HCl. The organic layer was dried (MgSO4) and the solvent removed under reduced pressure. Chromatography of the crude oil on 200 g of silica gel (230-400 mesh) using 0%-5% ethyl acetate in methylene chloride as the eluent gave 2-butyl-benzofuran-3-carboxylic acid benzyl-(6-hydroxy-naphthalen-2-ylmethyl)-amide (0.8164 g, 65%) as a light yellow solid, mp 160-164° C.

후처리

  1. additionAfter the addition the reaction
  2. customThe solid present was removed by filtration
  3. concentrationthe filtrate concentrated under reduced pressure
  4. customto give a brown oil
  5. extractionextracted with 1N HCl
  6. dry with materialThe organic layer was dried (MgSO4)
  7. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-89dbd9c1034b403ebb93356ea9eeb75c
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06589970B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트