Sodium Hydroxide → 4-(4-formylphenoxy)butanoic Acid

HRID 1360995ノート

反応式

HRID 1360995 の反応式
C([O:3][C:4](=[O:17])[CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:14]=[CH:13][C:12]([CH:15]=[O:16])=[CH:11][CH:10]=1)C.[OH-].[Na+]>CO>[CH:15]([C:12]1[CH:13]=[CH:14][C:9]([O:8][CH2:7][CH2:6][CH2:5][C:4]([OH:17])=[O:3])=[CH:10][CH:11]=1)=[O:16]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 15517709Ethyl 4-(4-formylphenoxy)butanoate

生成物 1

HCID 35191904-(4-formylphenoxy)butanoic Acid収率 91.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-(4-Formylphenoxy)butyric acid ethyl ester (19.6 g, 75 mmol) was dissolved in methanol (250 mL) and 1N sodium hydroxide (100 mL) was added and the resulting mixture was stirred at room temperature for 16 hours. The organic solvent was evaporated in vacuo (40° C., 120 mBar) and the residue was acidified with 1N hydrochloric acid (110 mL). The mixture was filtered and washed with water and dried in vacuo to afford 14.3 g (91%) 4-(4-formylphenoxy)butyric acid as a solid. 1H-NMR (DMSO-d6): δ 1.99 (2H, p), 2.42 (2H, t), 4.13 (2H, t), 7.14 (2H, d), 7.88 (2H, d), 9.90 (1H, s), 12.2 (1H, bs). HPLC-MS (Method A): m/z=209 (M+1); Rt=2.19 min.

後処理

  1. customThe organic solvent was evaporated in vacuo (40° C., 120 mBar)
  2. filtrationThe mixture was filtered
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-e4414adef0194a80a6bf8b5aeac05f7c
出典データセット
uspto-grants-2011_02
特許番号
US07879893B2

反応ノート

読み込み中…