Stannous chloride dihydrate → HCID 59625705、化合物

HRID 468175ノート

反応式

HRID 468175 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:18]=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[CH:11][C:10]=2[N+:19]([O-])=O)=[CH:4][CH:3]=1.O.O.Cl[Sn]Cl.C([O-])(O)=O.[Na+]>CCO>[NH2:19][C:10]1[CH:11]=[C:12]([CH:17]=[CH:18][C:9]=1[NH:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=1)[C:13]([O:15][CH3:16])=[O:14]

参加物

5

反応物 3

HCID 61436Stannous chloride dihydrateHCID 516892Sodium BicarbonateHCID 59625834HCID 59625834、化合物

生成物 1

HCID 59625705HCID 59625705、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

A mixture of 60c (1.4 g, 4.8 mmol) and SnCl2.2H2O (4.9 g, 21.7 mmol) in EtOH (50 mL) was stirred at 80° C. After 4 h, the mixture was cooled to room temperature and was slowly added to saturated aqueous NaHCO3. The solid was filtered and washed with H2O. The solid was triturated with EtOAc and the filtrate was concentrated. The crude product 60d was used in the next reaction without purification. MS m/z (M+H+) 261.1.

後処理

  1. temperaturethe mixture was cooled to room temperature
  2. filtrationThe solid was filtered
  3. washwashed with H2O
  4. customThe solid was triturated with EtOAc
  5. concentrationthe filtrate was concentrated
  6. customThe crude product 60d was used in the next reaction without purification

出典と根拠

ORDレコード
ord-620426c5d6ed4b1984a76f3f8c9c1380
出典データセット
uspto-grants-2014_01
特許番号
US08623858B2

反応ノート

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