Sodium Hydroxide → 2,5-Bis(benzyloxy)phenol

HRID 31213ノート

反応式

HRID 31213 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:10]=1[O:23]C(=O)C)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[CH:11][C:10]=1[OH:23])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

実験手順

A solution of acetic acid 2,5-bis(benzyloxy)phenyl ester (1.85 g) and 5M sodium hydroxide solution (10.6 ml) in ethanol (11 ml) was heated under reflux for 6.5 hrs. After ethanol was evaporated under reduced pressure the clear solution was made acidic with diluted hydrochloric acid. The precipitated product was collected by filtration, washed with cold water and dried under reduced pressure. Yield is 0.56 g. 1H NMR (DMSO-d6) δ=4.97 (s, 2H), 5.01 (s, 2H), 6.34 (dd, J=3.1, 8.8 Hz, 1H), 6.49(d, J=3.1 Hz, 1H), 6.85 (d, J=8.8 Hz, 1H), 7.28-7.46 (m, 10H), 9.1 (br s, 1H).

後処理

  1. temperatureunder reflux for 6.5 hrs
  2. customAfter ethanol was evaporated under reduced pressure the clear solution
  3. filtrationThe precipitated product was collected by filtration
  4. washwashed with cold water
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-1109bf4f454b4714b0b8984e3b4cffa9
出典データセット
uspto-grants-2008_09
特許番号
US07425568B2

反応ノート

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