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Lithium Hydroxide → {Tert-butyl-[3-(4',5'-difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-amino}-acetic acid

HRID 1665257
ノート
印刷プレビュー

反応式

HRID 1665257 の反応式
C([O:3][C:4](=[O:37])[CH2:5][N:6]([C:11](=[O:36])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][O:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]3[CH:31]=[C:30]([F:32])[C:29]([F:33])=[CH:28][C:27]=3[O:34][CH3:35])=[CH:22][CH:21]=2)[CH:13]=1)[C:7]([CH3:10])([CH3:9])[CH3:8])C.[Li+].[OH-]>C1COCC1.O>[C:7]([N:6]([CH2:5][C:4]([OH:37])=[O:3])[C:11](=[O:36])[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH2:18][O:19][C:20]2[CH:25]=[CH:24][C:23]([C:26]3[CH:31]=[C:30]([F:32])[C:29]([F:33])=[CH:28][C:27]=3[O:34][CH3:35])=[CH:22][CH:21]=2)[CH:13]=1)([CH3:10])([CH3:8])[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 67152350{[3-(4',5'-Difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-tert-butyl-amino}-acetic acid ethyl ester

生成物 1

HCID 52933305{Tert-butyl-[3-(4',5'-difluoro-2'-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-amino}-acetic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of {[3-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-tert-butyl-amino}-acetic acid ethyl ester (11.6 g, 23.3 mmol) in THF (500 mL) was treated with a solution LiOH (2.8 g, 116.7 mmol) in water (500 mL) at room temperature for 12 h. THF was then removed by evaporation. The mixture was then poured into ice and carefully acidified with dilute HCl to pH-1. The precipitate was collected by filtration, washed with water, and dried in vacuum to afford {tert-butyl-[3-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-benzoyl]-amino}-acetic acid as a white solid, 10.6 g (94%). LC-MS (ES) calculated for C27H27F2NO5, 483; found m/z 484 [M+H]+.

後処理

  1. customTHF was then removed by evaporation
  2. additionThe mixture was then poured into ice
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customdried in vacuum

出典と根拠

ORDレコード
ord-15158f27018d43fe824ed7558625c1e2
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039495B2

反応ノート

読み込み中…

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