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Hydrazine hydrate (1:1) → HCID 21190259、化合物

HRID 619515
ノート
印刷プレビュー

反応式

HRID 619515 の反応式
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7]([S:13][CH2:14][CH2:15][CH2:16][CH2:17][N:18]1C(=O)C2=CC=CC=C2C1=O)=[N:8]3.O.NN>C(O)C>[NH2:18][CH2:17][CH2:16][CH2:15][CH2:14][S:13][C:7]1[C:6]2=[C:2]([CH3:1])[N:3]=[C:4]3[N:5]2[C:9](=[CH:10][CH:11]=[CH:12]3)[N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 211900953-Methyl-[4-(phthalimido)butan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene

生成物 1

HCID 21190259HCID 21190259、化合物収率 72.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a suspension of 3.90 g (10.0 mmol) of 3-methyl-[4-(phthalimido)butan-1-ylthio]-1,4,7b-triazacyclopent[cd]indene in 70 ml of ethanol was added 1.50 g (30.0 mmol) of hydrazine monohydrate. The mixture was heated for 2 hours under reflux. After cooling the resulting precipitates were filtered off. The filtrate was concentrated to give the residue, water was added, extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, then the solvent was distilled off to give 1.89 g of the desired compound (72.7%, pale brown solid)

後処理

  1. temperatureThe mixture was heated for 2 hours
  2. temperatureunder reflux
  3. temperatureAfter cooling the resulting
  4. customprecipitates
  5. filtrationwere filtered off
  6. concentrationThe filtrate was concentrated
  7. customto give the residue, water
  8. additionwas added
  9. extractionextracted with chloroform
  10. dry with materialThe extract was dried over anhydrous magnesium sulfate
  11. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-5003700007a14b47aa882275691e8abe
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05958942

反応ノート

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