Ammonium Chloride → HCID 68466596、化合物

HRID 1927711ノート

反応式

HRID 1927711 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:11]=[C:12]([CH2:26][C:27]([O:29][CH3:30])=[O:28])[CH:13]=[CH:14][C:15]=1[O:16][C:17]1[CH:22]=[CH:21][C:20]([N+:23]([O-])=O)=[CH:19][CH:18]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Cl-].[NH4+]>C1COCC1.C(OCC)(=O)C.C(=O)(O)[O-].[Na+].[Zn]>[NH2:23][C:20]1[CH:19]=[CH:18][C:17]([O:16][C:15]2[CH:14]=[CH:13][C:12]([CH2:26][C:27]([O:29][CH3:30])=[O:28])=[CH:11][C:10]=2[CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[CH:22][CH:21]=1

参加物

7

反応物 2

HCID 25517Ammonium ChlorideHCID 68464706HCID 68464706、化合物

生成物 1

HCID 68466596HCID 68466596、化合物収率 100.2%

試薬・触媒・溶媒 4

HCID 23994Zinc触媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

Methyl 2-(3-((tert-butoxycarbonyl)aminomethyl)-4-(4-nitrophenoxy)phenyl)acetate (242 mg, 0.581 mmol) was diluted with THF (3 mL) followed by the addition of Zn dust (38.0 mg, 0.581 mmol). About 2 mL of saturated ammonium chloride was added dropwise. After stirring the reaction for 10 minutes, the reaction mixture was diluted with ethyl acetate and saturated sodium bicarbonate. The layers were separated and the organic layer was dried over MgSO4, filtered and concentrated to yield 225 mg of methyl 2-(4-(4-aminophenoxy)-3-((tert-butoxycarbonyl)aminomethyl)phenyl)acetate.

後処理

  1. customthe reaction for 10 minutes
  2. customThe layers were separated
  3. dry with materialthe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8310c631adae4ea38a20b0f613116da2
出典データセット
uspto-grants-2012_05
特許番号
US08183289B2

反応ノート

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