HCID 66767215, 화합물 → HCID 66767283, 화합물

HRID 2195525노트

반응식

HRID 2195525 반응식
[F:1][C:2]1[CH:30]=[C:29]([N+:31]([O-])=O)[CH:28]=[CH:27][C:3]=1[O:4][C:5]1[CH:6]=[C:7]2[C:11](=[CH:12][C:13]=1[C:14]1[CH:15]=[N:16][N:17]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH:18]=1)[N:10]([CH3:26])[N:9]=[CH:8]2>[Pd].C1COCC1>[NH2:31][C:29]1[CH:28]=[CH:27][C:3]([O:4][C:5]2[CH:6]=[C:7]3[C:11](=[CH:12][C:13]=2[C:14]2[CH:15]=[N:16][N:17]([C:19]([O:21][C:22]([CH3:24])([CH3:25])[CH3:23])=[O:20])[CH:18]=2)[N:10]([CH3:26])[N:9]=[CH:8]3)=[C:2]([F:1])[CH:30]=1

참가 물질

4

반응물 1

HCID 66767215HCID 66767215, 화합물

생성물 1

HCID 66767283HCID 66767283, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매2회HCID 8028Tetrahydrofuran용매

반응 조건

온도
35 °C

실험 절차

To a 3 gallon tank is added tert-butyl 4-(5-(2-fluoro-4-nitrophenoxy)-1-methyl-1H-indazol-6-yl)-1H-pyrazole-1-carboxylate (433.0 g, 952.8 mmol) followed by THF (6.5 L) and Pd/C (21.65 g, 10% Pd/C and 21.65 g, 5% Pd/C). The mixture is heated to 35° C. under hydrogen gas for 2 hours. The reaction is then cooled to RT and allowed to stir under hydrogen gas overnight, then is heated to 40° C. under hydrogen gas for seven hours. An additional 2 g Pd/C (1 g, 10% Pd/C and 1 g, 5% Pd/C) is added and stirred under hydrogen gas for another hour and cooled to RT. The mixture is again stirred under hydrogen gas overnight and the reaction is completed. The mixture is filtered over a combination of GFF® and Watman® paper. The filtrate is concentrated to a slightly yellow solid (446 g, 110% recovery).

후처리

  1. temperatureThe reaction is then cooled to RT
  2. temperatureis heated to 40° C. under hydrogen gas for seven hours
  3. stirringstirred under hydrogen gas for another hour
  4. temperaturecooled to RT
  5. stirringThe mixture is again stirred under hydrogen gas overnight
  6. filtrationThe mixture is filtered over a combination of GFF® and Watman® paper
  7. concentrationThe filtrate is concentrated to a slightly yellow solid (446 g, 110% recovery)

출처 및 근거

ORD 기록
ord-9542daac59774a3fb68aa2ceac3fcb45
출처 데이터셋
uspto-grants-2012_12
특허 번호
USRE043878E1

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