Methacrylic Acid → 3-Hydroxy-1-adamantyl acrylate

HRID 1019479

반응식

HRID 1019479 반응식
[C:1]([OH:6])(=[O:5])[C:2](C)=[CH2:3].[OH:7][C:8]12[CH2:17][CH:12]3[CH2:13][CH:14]([CH2:16][C:10](C=C(C)C([O-])=O)([CH2:11]3)[CH2:9]1)[CH2:15]2.C1C2C(=CC3C(C=2COC(=O)C(C)=C)=CC=CC=3)C=CC=1.CC(C)C#N>O1CCCC1>[CH2:3]=[CH:2][C:1]([O:6][C:10]12[CH2:9][C:8]3([OH:7])[CH2:17][CH:12]([CH2:13][CH:14]([CH2:15]3)[CH2:16]1)[CH2:11]2)=[O:5]

참가 물질

6

반응물 4

HCID 4093Methacrylic AcidHCID 6559IsobutyronitrileHCID 36187549-Anthrylmethyl methacrylateHCID 1317313693-Hydroxy-1 adamantylmethacrylate

생성물 1

HCID 222287903-Hydroxy-1-adamantyl acrylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a mixture of methacrylic acid (0.775 g, 9 mmol), 3-hydroxy-1 adamantylmethacrylate (1.42 g, 6 mmol), 9-anthrylmethylmethacrylate (1.38 g, 5 mmol) in 20 mL of tetrahydrofuran (THF) was added 2,2′-azobis(2-methylpropionitrile (0.16 g, 1 mmol). The resulting solution was purged by nitrogen for 30 minutes before it was heats to 72° C. for 18 hours under nitrogen. The solution was then cooled to room temperature and added drop-wise into 400 mL of de-ionized water. The solid was filtered with a frit funnel, washed with water (2×200 ml) and dried in a vacuum oven at 50° C. for 24 hours to afford 3.1 gram of P1 as white solid.

후처리

  1. additionwas added
  2. customThe resulting solution was purged by nitrogen for 30 minutes before it
  3. customto 72° C.
  4. customfor 18 hours
  5. additionadded drop-wise into 400 mL of de-ionized water
  6. filtrationThe solid was filtered with a frit funnel
  7. washwashed with water (2×200 ml)
  8. customdried in a vacuum oven at 50° C. for 24 hours
  9. customto afford 3.1 gram of P1 as white solid

출처 및 근거

ORD 기록
ord-77bd4faca56641d7918889d62309813e
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08715907B2

연결된 노트

불러오는 중…