Ammonium Chloride → HCID 68466596, 화합물

HRID 1927711노트

반응식

HRID 1927711 반응식
[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

참가 물질

7

반응물 2

HCID 25517Ammonium ChlorideHCID 68464706HCID 68464706, 화합물

생성물 1

HCID 68466596HCID 68466596, 화합물수율 100.2%

시약·촉매·용매 4

HCID 23994Zinc촉매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8310c631adae4ea38a20b0f613116da2
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08183289B2

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