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Lithium Hydroxide → 4-Amino-3-iodobenzoic Acid

HRID 2281180
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HRID 2281180 반응식
[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]
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참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 4104649Methyl 4-amino-3-iodobenzoate

생성물 1

HCID 164614-Amino-3-iodobenzoic Acid수율 98.6%

시약·촉매·용매 1

HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

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.

후처리

  1. distillationThe dioxane was distilled off in vacuo
  2. filtrationThe precipitate was filtered off with suction
  3. washwashed with water

출처 및 근거

ORD 기록
ord-26e48a7e62ea4df790bada8bd6c49550
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09139579B2

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