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

Hydrochloric Acid → HCID 22375175, 화합물

HRID 1956091
노트
인쇄 미리보기

반응식

HRID 1956091 반응식
[CH2:1]([CH:6]1[CH2:11][CH2:10][CH:9]([CH:12]2[CH2:17][CH2:16][CH:15]([OH:18])[CH2:14][CH2:13]2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].[H-].[Na+].Br[CH2:22][C:23]1([CH2:29][CH3:30])OCCC[O:24]1.BrCC(=O)CC.Cl>C1COCC1.C1(C)C=CC=CC=1.CN(C=O)C>[CH2:1]([CH:6]1[CH2:11][CH2:10][CH:9]([CH:12]2[CH2:17][CH2:16][CH:15]([O:18][CH2:22][C:23](=[O:24])[CH2:29][CH3:30])[CH2:14][CH2:13]2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 131561-Bromo-2-butanoneHCID 24758Sodium hydrideHCID 31262334'-Pentyl(1,1'-bicyclohexyl)-4-olHCID 22375208HCID 22375208, 화합물

생성물 1

HCID 22375175HCID 22375175, 화합물수율 65%

시약·촉매·용매 3

HCID 1140
Toluene
용매
2회
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매3회

실험 절차

A solution of 25.2 g (0.1 mol) of 4-(4-pentylcyclohexyl) cyclohexanol in 50 ml of THF was added dropwise to a mixture of 5.2 g (0.11 mol) of sodium hydride and 20 ml of THF at a temperature of lower than 10° C. Then, 50 ml of DMF was further added and stirred for 1 hour at a room temperature. While keeping inside of the reaction system at a temperature of lower than 0°C., a solution of 21 g (0.1 mol) of 2-bromomethyl-2-ethyl-1,3-dioxane derived from commercially available 1-bromo-2-butanone in 50 ml of THF was added dropwise, and stirred for 2 hours at a room temperature and then for 2 hours at 50° C. This solution was added with 50 ml of 6N hydrochloric acid, stirred for 1 hour at 50° C., added with 200 ml of toluene, and extracted. The organic layer was washed once with an aqueous solution saturated with potassium carbonate and twice with water, and dried over anhydrous magnesium sulfate. After the anhydrous magnesium sulfate was separated, the solvent was distilled off under a reduced pressure, and the residue thus obtained was subjected to a silica gel column chromatography (eluate: toluene) to obtain 20.9 g (yield 65%) of 4-(4-pentylcyclohexyl)-(2-oxobutyloxy)cyclohexane.

후처리

  1. customlower than 0°C.
  2. additionwas added dropwise
  3. stirringstirred for 2 hours at a room temperature
  4. waitfor 2 hours at 50° C
  5. stirringstirred for 1 hour at 50° C.
  6. extractionextracted
  7. washThe organic layer was washed once with an aqueous solution saturated with potassium carbonate and twice with water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customAfter the anhydrous magnesium sulfate was separated
  10. distillationthe solvent was distilled off under a reduced pressure
  11. customthe residue thus obtained

출처 및 근거

ORD 기록
ord-ec550bf550a44a51be783b946cc4f55d
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05779936

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트