Thiourea → HCID 86665174、化合物

HRID 1893721ノート

反応式

HRID 1893721 の反応式
[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13](=O)[CH2:14]Br)[CH:10]=[N:9]2)=[CH:5][CH:4]=1.[NH2:19][C:20]([NH2:22])=[S:21]>CC(C)=O>[CH3:1][O:2][C:3]1[CH:18]=[CH:17][C:6]([CH2:7][N:8]2[CH:12]=[C:11]([C:13]3[N:19]=[C:20]([NH2:22])[S:21][CH:14]=3)[CH:10]=[N:9]2)=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 2723790ThioureaHCID 866423312-Bromo-1-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)ethanone

生成物 1

HCID 86665174HCID 86665174、化合物収率 83.9%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

According to Scheme 6, Step 1: A solution of 1-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-2-bromoethanone (9.70 mmol, 3.00 g) and of thiourea (9.70 mmol, 739 mg) in acetone (20 mL) was stirred under reflux for 1 hour. After filtration and evaporation of the filtrate, the white solid was partitioned between EtOAc and a saturated solution of Na2CO3. The aqueous phase was extracted with EtOAc. The organic phase was dried over Na2SO4, was filtered and was concentrated to yield 4-(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)thiazol-2-amine (8.14 mmol, 2.33 g) as an orange foam.

後処理

  1. temperatureunder reflux for 1 hour
  2. filtrationAfter filtration and evaporation of the filtrate
  3. customthe white solid was partitioned between EtOAc
  4. extractionThe aqueous phase was extracted with EtOAc
  5. dry with materialThe organic phase was dried over Na2SO4
  6. filtrationwas filtered
  7. concentrationwas concentrated

出典と根拠

ORDレコード
ord-72713a5767034d60b0ee9f0e8901310c
出典データセット
uspto-grants-2013_08
特許番号
US08513252B2

反応ノート

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