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

Phenol → HCID 86710600, 화합물

HRID 1027203
노트
인쇄 미리보기

반응식

HRID 1027203 반응식
C1(O)C=CC=CC=1.C([O-])([O-])=O.[Cs+].[Cs+].[CH2:14]([O:21][C:22]1[CH:31]=[C:30]2[C:25]([CH:26]=[CH:27][C:28]([OH:32])=[CH:29]2)=[CH:24][C:23]=1[Br:33])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.Br[CH2:35][CH2:36][CH2:37][O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1.[Na+].[I-]>CC(C)=O.CCOC(C)=O>[CH2:14]([O:21][C:22]1[C:23]([Br:33])=[CH:24][C:25]2[C:30]([CH:31]=1)=[CH:29][C:28]([O:32][CH2:35][CH2:36][CH2:37][O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[CH:27][CH:26]=2)[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 996PhenolHCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 2776064Benzyl 3-Bromopropyl EtherHCID 748928207-(Benzyloxy)-6-bromonaphthalen-2-ol

생성물 1

HCID 86710600HCID 86710600, 화합물수율 60%

시약·촉매·용매 2

HCID 180
Acetone
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

Following GENERAL METHOD 5-1 for phenol alkylation, Cs2CO3 (485 mg, 1.489 mmol) was added to a solution of 7-(benzyloxy)-6-bromonaphthalen-2-ol (490 mg, 1.489 mmol) in acetone (14.90 mL) at RT. The reaction mixture was stirred for 5 min then ((3-bromopropoxy)methyl)benzene (682 mg, 2.98 mmol) was added, followed by addition of NaI (446 mg, 2.98 mmol). The reaction mixture was heated to 60° C. and stirred overnight, then filtered, washed with acetone and concentrated in vacuo. The resulting residue was partitioned between Et2O (60 mL) and water (20 mL). After separation, the organic layer was washed with saturated aq. sodium sulfite solution (20 mL), 2 M Na2CO3, and brine. The organic layer was then dried over MgSO4, filtered, and concentrated in vacuo. Silica gel chromatography (10-60% EtOAc/heptane) afforded 3-(benzyloxy)-6-(3-(benzyloxy)propoxy)-2-bromonaphthalene (422 mg, 0.884 mmol, 60% yield) as a white solid (eluting at 30% EtOAc). LCMS Rt=1.81 min (condition C); LCMS (M+1)=479.9.

후처리

  1. stirringstirred overnight
  2. filtrationfiltered
  3. washwashed with acetone
  4. concentrationconcentrated in vacuo
  5. customThe resulting residue was partitioned between Et2O (60 mL) and water (20 mL)
  6. customAfter separation
  7. washthe organic layer was washed with saturated aq. sodium sulfite solution (20 mL), 2 M Na2CO3, and brine
  8. dry with materialThe organic layer was then dried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo
  11. customSilica gel chromatography (10-60% EtOAc/heptane) afforded

출처 및 근거

ORD 기록
ord-30b2cd6d0bc647359469a82493569f6d
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729263B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트