Ethanol → HCID 67259831、化合物

HRID 79259ノート

反応式

HRID 79259 の反応式
[CH2:1]([N:8]1[C:16]2[C:11](=[C:12]([N+:17]([O-])=O)[CH:13]=[CH:14][CH:15]=2)[C:10]([CH2:20][CH3:21])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+].C(O)C>[Fe].O>[CH2:1]([N:8]1[C:16]2[CH:15]=[CH:14][CH:13]=[C:12]([NH2:17])[C:11]=2[C:10]([CH2:20][CH3:21])=[N:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 702EthanolHCID 25517Ammonium ChlorideHCID 67259581HCID 67259581、化合物

生成物 1

HCID 67259831HCID 67259831、化合物収率 97%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
85 °C

実験手順

A mixture of 1-benzyl-3-ethyl-4-nitro-1H-indazole (46.0 mg, 0.164 mmol), iron powder (91.3 mg, 1.64 mmol) and ammonium chloride (4.4 mg, 0.082 mmol) was stirred in a 4:1 mixture of ethanol and water (5 mL) with heating to 85° C. for 60 minutes. The solvent was removed under reduced pressure. Ethyl acetate (4 mL) and triethylamine (1 mL) was added and the mixture was heated for 15 minutes at 85° C. After cooling, the mixture was filtered through glass fiber filter paper, rinsing with methanol, dichloromethane and ethyl acetate. The filtrate was concentrated under reduced pressure to provide 1-benzyl-3-ethyl-1H-indazol-4-amine as an oil (40 mg).

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionEthyl acetate (4 mL) and triethylamine (1 mL) was added
  3. temperaturethe mixture was heated for 15 minutes at 85° C
  4. temperatureAfter cooling
  5. filtrationthe mixture was filtered through glass fiber
  6. filtrationfilter paper
  7. washrinsing with methanol, dichloromethane and ethyl acetate
  8. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-e6fae5492da24fd1b1c3bbc42bdb3962
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

反応ノート

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