Hydrochloric Acid → HCID 67153767、化合物

HRID 547862ノート

反応式

HRID 547862 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([N+:23]([O-])=O)[CH:18]=3)=[CH:11][CH:10]=2)=[C:4]([O:26][CH3:27])[CH:3]=1.[ClH:28]>CCOC(C)=O.CCO.[Pd]>[ClH:28].[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([C:9]2[CH:10]=[CH:11][C:12]([O:15][CH2:16][C:17]3[CH:18]=[C:19]([NH2:23])[CH:20]=[CH:21][CH:22]=3)=[CH:13][CH:14]=2)=[C:4]([O:26][CH3:27])[CH:3]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 582877964,5-Difluoro-2-methoxy-4'-(3-nitro-benzyloxy)-biphenyl

生成物 1

HCID 67153767HCID 67153767、化合物収率 95%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4,5-difluoro-2-methoxy-4′-(3-nitro-benzyloxy)-biphenyl (300 mg, 0.808 mmol) and 10% Pd/C (45 mg) in EtOAc (2 mL), EtOH (13 mL) and 6N HCl (150 uL) was hydrogenated at 50 psi for 1.5 hrs. The reaction mixture was filtered through Celite and evaporated to dryness to give 289 mg (95%) of 3-(4′,5′-difluoro-2′-methoxy-biphenyl-4-yloxymethyl)-phenylamine hydrochloride. LC-MS (ES) calculated for C20H17F2NO2, 341.36; found m/z 342 [M+H]+.

後処理

  1. filtrationThe reaction mixture was filtered through Celite
  2. customevaporated to dryness

出典と根拠

ORDレコード
ord-254db79895374d97a2cbb2c074e740d9
出典データセット
uspto-grants-2011_05
特許番号
US07939569B1

反応ノート

読み込み中…