Ammonium formate → HCID 68467096, 화합물

HRID 132925

반응식

HRID 132925 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:19]([N+:20]([O-])=O)=[CH:18][CH:17]=[CH:16][C:15]=2[Cl:23])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([O-])=O.[NH4+].CC(C)=O.C(Cl)Cl>CO.[Pd]>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:15]([Cl:23])=[CH:16][CH:17]=[CH:18][C:19]=2[NH2:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 3

HCID 2723923Ammonium formateHCID 21584124Propan-2-one--dichloromethane (1/1)HCID 587677041-Boc-4-(2-chloro-6-nitrophenyl)piperazine

생성물 1

HCID 68467096HCID 68467096, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

반응 조건

온도
65 °C

실험 절차

A solution of 342 mg (1 mmol) of 4-(2-chloro-6-nitro-phenyl)-piperazine-1-carboxylic acid tert-butyl ester in 5.0 mL of MeOH was treated with 630 mg (10 mmol, 10 eq) of ammonium formate and a catalytic amount of 10% Pd—C (34 mg). The reaction mixture was stirred at 65° C. for 30 min. The reaction mixture was then filtered through a pad of celite and concentrated to obtain a yellow solid. TLC (silica, 5% acetone/CH2Cl2): Rf=0.40. MS (electrospray): exact mass calculated for C15H22ClN3O2, 311.14; m/z found, 312.1 [M+H]+.

후처리

  1. filtrationThe reaction mixture was then filtered through a pad of celite
  2. concentrationconcentrated
  3. customto obtain a yellow solid

출처 및 근거

ORD 기록
ord-a0500cb5a08642e4a47fcd628ad2a8d0
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388011B2

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