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

4-[4-(1-Adamantyl)-phenoxy]-2-butenoic acid → 4-[4-(1-Adamantyl)-phenoxy]butyric acid

HRID 258984
노트
인쇄 미리보기

반응식

HRID 258984 반응식
[C:1]12([C:11]3[CH:23]=[CH:22][C:14]([O:15][CH2:16][CH:17]=[CH:18][C:19]([OH:21])=[O:20])=[CH:13][CH:12]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.C12(C3C=CC(OC=CCC(O)=O)=CC=3)CC3CC(CC(C3)C1)C2.[H][H]>[Pd].CO>[C:1]12([C:11]3[CH:12]=[CH:13][C:14]([O:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=[O:20])=[CH:22][CH:23]=3)[CH2:8][CH:7]3[CH2:9][CH:3]([CH2:4][CH:5]([CH2:6]3)[CH2:10]1)[CH2:2]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 544821354-[4-(1-Adamantyl)-phenoxy]-2-butenoic acidHCID 545391144-[4-(1-Adamantyl)-phenoxy]-3-butenoic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 214251534-[4-(1-Adamantyl)-phenoxy]butyric acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887
Methanol
용매

실험 절차

A solution of 0.9 g of the mixture of 4-[4-(1-adamantyl)-phenoxy]-2-butenoic acid and 4-[4-(1-adamantyl)-phenoxy]-3-butenoic acid is 30 ml of absolute methanol is hydrogenated with 0.3 g of palladium (5% strength on charcoal) until 1 equivalent of hydrogen has been taken up (normal pressure, about 25° C). The catalyst is then filtered off, and the filtrate is mixed with 10 ml of 2 N sodium hydroxide solution and left to stand for 24 hours at about 25° C. It is then evaporated in vacuo to half its volume. The evaporation residue is partitioned between 50 ml of 2 N hydrochloric acid and 3 times 50 ml of methylene chloride. The organic phases are washed until neutral, dried over sodium sulphate and evaporated in vacuo. Crystallisation of the evaporation residue from ethanol gives 4-[4-(1-adamantyl)-phenoxy]butyric acid of melting point 170°-172° C.

후처리

  1. custom(normal pressure, about 25° C)
  2. filtrationThe catalyst is then filtered off
  3. additionthe filtrate is mixed with 10 ml of 2 N sodium hydroxide solution
  4. waitleft
  5. customIt is then evaporated in vacuo to half its volume
  6. customThe evaporation residue is partitioned between 50 ml of 2 N hydrochloric acid and 3 times 50 ml of methylene chloride
  7. washThe organic phases are washed until neutral,
  8. dry with materialdried over sodium sulphate
  9. customevaporated in vacuo
  10. customCrystallisation of the evaporation residue from ethanol

출처 및 근거

ORD 기록
ord-c5b93fae33c14131815bb0db3b43ad8c
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04035413

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트