3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole → 3-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

HRID 1020947노트

반응식

HRID 1020947 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-])=O)[CH:16]=3)[N:11]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1>CO.C1(C)C=CC=CC=1.[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([NH2:18])[CH:16]=3)[N:11]([C:21]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1

참가 물질

4

반응물 1

HCID 673446273-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole

생성물 1

HCID 583720003-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 21867641Toluene methanol용매

실험 절차

To the stirred suspension of 3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 4BV (5.125 g, 10.0 mmole) in MeOH/toluene (50 mL/50 mL) was added 10% Pd/C (Degussa type, 0.5 g) at r.t. under dry N2 gas. The mixture was degassed and was stirred under a balloon inflated with H2 gas overnight. The catalyst was filtered through microfiber filter and was washed with MeOH and CH2Cl2. The filtrate was evaporated to dryness and a brown solid 5BV was obtained (5.0 g).

후처리

  1. customThe mixture was degassed
  2. custominflated with H2 gas overnight
  3. filtrationThe catalyst was filtered through microfiber
  4. filtrationfilter
  5. washwas washed with MeOH and CH2Cl2
  6. customThe filtrate was evaporated to dryness
  7. customa brown solid 5BV was obtained (5.0 g)

출처 및 근거

ORD 기록
ord-311c9f53991841e99af52dc0f4531318
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716483B2

반응 노트

불러오는 중…