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Hydrazine hydrate (1:1) → 2-amino-N-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]acetamide

HRID 1247833
ノート
印刷プレビュー

反応式

HRID 1247833 の反応式
O.NN.O=C1C2C(=CC=CC=2)C(=O)[N:6]1[CH2:15][C:16]([NH:18][C:19]1[CH:20]=[N:21][N:22]([CH3:44])[C:23]=1[NH:24][C:25]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:17]>C(O)C.O1CCCC1>[NH2:6][CH2:15][C:16]([NH:18][C:19]1[CH:20]=[N:21][N:22]([CH3:44])[C:23]=1[NH:24][C:25]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1)[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)=[O:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 219045342-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-N-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]acetamide

生成物 1

HCID 219045762-amino-N-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]acetamide収率 81.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
70 °C

実験手順

Hydrazine monohydrate (1.46 ml) was added to a solution of 2-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-N-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]acetamide (5.42 g) in ethanol (108 ml) and tetrahydrofuran (54 ml) at room temperature, and the mixture was stirred at 70° C. for 2 hours. The reaction mixture was cooled to 0° C., and the insoluble materials were removed by filtration. The filtrate was concentrated in vacuo. The residue was triturated with diisopropyl ether, collected by filtration and dried in vacuo to give 2-amino-N-[1-methyl-5-(tritylamino)-1H-pyrazol-4-yl]acetamide (3.37 g) as a solid. This product was used in the next step without further purification.

後処理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. customthe insoluble materials were removed by filtration
  3. concentrationThe filtrate was concentrated in vacuo
  4. customThe residue was triturated with diisopropyl ether
  5. filtrationcollected by filtration
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-8b6ef869bf6548c582f6ad9026a37f7d
出典データセット
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07129232B2

反応ノート

読み込み中…

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