Lithium Hydroxide → 4-Amino-3-iodobenzoic Acid
反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8]C)=[O:7])=[CH:4][C:3]=1[I:12].[OH-].[Li+]>O1CCOCC1.O>[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[I:12]参加物
4
実験手順
A solution of 3.00 g (10.8 mmol) of methyl 4-amino-3-iodobenzoate and 1.30 g (54.1 mmol) of lithium hydroxide in 150 ml of a dioxane/water mixture (1:1) was stirred at room temperature for 6 h. The dioxane was distilled off in vacuo, and the remaining aqueous phase was adjusted to pH 5 with 1 M hydrochloric acid. The precipitate was filtered off with suction and washed with water. 2.80 g (98%) of the title compound were obtained as a solid.
後処理
- distillationThe dioxane was distilled off in vacuo
- filtrationThe precipitate was filtered off with suction
- washwashed with water
出典と根拠
- ORDレコード
- ord-f66deb25d8444913ab070ad0765ffe80
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07256288B2
反応ノート
読み込み中…