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HCID 21834217、化合物 → HCID 57203651、化合物

HRID 1708994
ノート
印刷プレビュー

反応式

HRID 1708994 の反応式
N[C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH2:8][CH:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1.N([O-])=[O:21].[Na+]>S(=O)(=O)(O)O.O>[OH:21][C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH2:8][CH:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1
参加物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 21834217HCID 21834217、化合物HCID 23668193Sodium Nitrite

生成物 1

HCID 57203651HCID 57203651、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 1118Sulfuric Acid溶媒2 回

実験手順

11.6 g of 5-amino-2,3-dihydro-N,N-dipropyl-3-benzothiophencarboxamide were dissolved in a mixture of 4 ml of conc. sulphuric acid and 40 ml of water. 3.1 g of sodium nitrite dissolved in 10 ml of water were added dropwise below 10° C. with stirring. After addition the mixture was stirred for further 0.5 hours. The diazonium solution was then added carefully to a pre-heated solution of 50 ml of conc. sulphuric acid in 40 ml of water at 115°-120° C. The resulting mixture was poured onto ice and subsequently extracted with dichloromethane. Yield of the title compound as a semicrystalline product: 8.7 g.

後処理

  1. additionwere added dropwise below 10° C.
  2. additionAfter addition the mixture
  3. stirringwas stirred for further 0.5 hours
  4. additionThe resulting mixture was poured onto ice
  5. extractionsubsequently extracted with dichloromethane

出典と根拠

ORDレコード
ord-a4337253bd404ffd934c3c68591c4702
出典データセット
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04946863

反応ノート

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