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Dimethylamine → N,N-Dimethyl-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazin-6-amine

HRID 1980088
ノート
印刷プレビュー

反応式

HRID 1980088 の反応式
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=1.[CH3:15][NH:16][CH3:17]>CO>[CH3:15][N:16]([CH3:17])[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=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 674DimethylamineHCID 133767996-Chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine

生成物 1

HCID 13376800N,N-Dimethyl-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazin-6-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture was prepared from 6 g of 6-chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine, 150 ml of methanol and 125 ml of 40% aqueous dimethylamine. This mixture was heated at reflux for 3 hours and then cooled. The precipitate which formed was separated by filtration and partitioned between methylene chloride and water. The organic layer was separated, dried over sodium sulfate, and concentrated to leave a residual solid. This was recrystallized from ethanol to give 6-dimethylamino-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine melting at about 239°-240° C.

後処理

  1. temperatureThis mixture was heated
  2. temperatureat reflux for 3 hours
  3. temperaturecooled
  4. customThe precipitate which formed
  5. customwas separated by filtration
  6. custompartitioned between methylene chloride and water
  7. customThe organic layer was separated
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated
  10. customto leave a residual solid
  11. customThis was recrystallized from ethanol

出典と根拠

ORDレコード
ord-df05722a5b8544f08714fcde3ed78591
出典データセット
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04485106

反応ノート

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