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HCID 1089054、化合物 → HCID 136006861、化合物

HRID 2052280
ノート
印刷プレビュー

反応式

HRID 2052280 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH:12]=[N:13][N:14]=[C:7]1[N:6]=[C:5]2[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[BH4-].[Na+]>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[CH:12]=[N:13][N:14]=[C:7]1[NH:6][CH:5]2[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=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 1089054HCID 1089054、化合物HCID 4311764Sodium borohydride

生成物 1

HCID 136006861HCID 136006861、化合物収率 45.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 2.6 g of 7-chloro-5-phenyl-s-triazolo[4,3-a]quinazoline in 100 ml of dimethylformamide was added 1 g of sodium borohydride. The mixture was stirred at room temperature overnight and then poured into ice-water. The resulting precipitate was collected by filtration, washed with water and dried. The so obtained solid was suspended in a mixture of 30 ml of methanol and 30 ml of concentrated hydrochloric acid, and the mixture was heated under reflux for 40 minutes. After cooling, the resulting mixture was neutralized with ammonia water. The precipitate formed was collected by filtration, washed with water, and recrystallized from methanol to give 1.2 g of 7-chloro-4,5-dihydro-5-phenyl-s-triazolo[4,3-a]quinazoline as colorless prisms, m.p. 241.5°-243.5° C.

後処理

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with water
  3. customdried
  4. additionThe so obtained solid was suspended in a mixture of 30 ml of methanol and 30 ml of concentrated hydrochloric acid
  5. temperaturethe mixture was heated
  6. temperatureunder reflux for 40 minutes
  7. temperatureAfter cooling
  8. customThe precipitate formed
  9. filtrationwas collected by filtration
  10. washwashed with water
  11. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-feaafe6cbb68417489bf69e93c5f923d
出典データセット
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04183932

反応ノート

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