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Water → HCID 178527906、化合物

HRID 1597237
ノート
印刷プレビュー

反応式

HRID 1597237 の反応式
[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13](=O)[NH:14][CH:15]=[N:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21].O>N1C=CC=CC=1>[CH2:1]([O:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13](=[S:21])[NH:14][CH:15]=[N:16]2)=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH: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

5

反応物 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 1357631107-(Benzyloxy)-3,4-dihydroquinazolin-4-one

生成物 1

HCID 178527906HCID 178527906、化合物収率 99%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A suspension of 7-benzyloxy-3,4-dihydroquinazolin-4-one (7 g, 28 mmol), (prepared as described for the starting material in Example 6), in pyridine (350 ml) containing phosphorus pentasulphide (12.5 g, 33 mmol) was heated at reflux for 8 hours. After cooling, the mixture was poured into water (1 liter). The precipitate was collected by filtration, and washed with water. The solid was dissolved in 6M sodium hydroxide and the solution was filtered. The filtrate was acidified to pH2 with 6M hydrochloric acid. The precipitate was collected by filtration, washed with water, and dried under vacuum at 60° C. to give 7-benzyloxy-3,4-dihydroquinazolin-4-thione (7.42 g, 99%).

後処理

  1. custom(prepared
  2. temperaturewas heated
  3. temperatureat reflux for 8 hours
  4. temperatureAfter cooling
  5. filtrationThe precipitate was collected by filtration
  6. washwashed with water
  7. dissolutionThe solid was dissolved in 6M sodium hydroxide
  8. filtrationthe solution was filtered
  9. filtrationThe precipitate was collected by filtration
  10. washwashed with water
  11. customdried under vacuum at 60° C.

出典と根拠

ORDレコード
ord-81454e966c694571947f14c84503f8c9
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06294532B1

反応ノート

読み込み中…

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