Sodium Hydroxide → HCID 20402696、化合物

HRID 1980265ノート

反応式

HRID 1980265 の反応式
[OH-:1].[Na+].Cl.[NH2:4]O.[C:6]([C:14]1[C:15]([NH:21][C:22](=[O:25])[CH2:23]I)=[CH:16][N:17]([CH3:20])[C:18]=1[CH3:19])(=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>O.C(O)C>[C:6]([C:14]1[C:15]([NH:21][C:22](=[O:25])[CH2:23][NH:4][OH:1])=[CH:16][N:17]([CH3:20])[C:18]=1[CH3:19])(=[O:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 20402707HCID 20402707、化合物

生成物 1

HCID 20402696HCID 20402696、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Sodium hydroxide (64 g) was added to a solution of hydroxylamine hydrochloride (111 g) in water (370 ml) and the obtained solution was diluted with ethanol (3500 ml). N-(4-benzoyl-1,5-dimethyl(1H)pyrrol-3-yl)-2-iodoacetamide (124.5 g) was then added and the obtained suspension was stirred under nitrogen stream for about 48 hours. The reaction mixture was filtered in order to remove the salts and the filtrate was concentrated to dryness at the pump. The residue was washed with a small amount of water and crystallized from ethyl acetate yielding 82.5 g of the compound of the title. M.p. 140°-42° C.

後処理

  1. filtrationThe reaction mixture was filtered in order
  2. customto remove the salts
  3. concentrationthe filtrate was concentrated to dryness at the pump
  4. washThe residue was washed with a small amount of water
  5. customcrystallized from ethyl acetate yielding 82.5 g of the compound of the title

出典と根拠

ORDレコード
ord-c344f08c91ec4804b2a17be78cd21e0f
出典データセット
uspto-grants-1985_04
特許番号
US04508730

反応ノート

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