Methacrylic Acid → 3-Hydroxy-1-adamantyl acrylate

HRID 576463

反応式

HRID 576463 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 222287903-Hydroxy-1-adamantyl acrylate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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 (0.24 g, 1.5 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.

後処理

  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

出典と根拠

ORDレコード
ord-ab777640358c424cb13edfe6d898c23f
出典データセット
uspto-grants-2015_05
特許番号
US09040225B2

関連ノート

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