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Dabco → 2,4-Diamino-6-(3,4-dichlorophenylsulfinyl)quinazoline

HRID 363766
ノート
印刷プレビュー

反応式

HRID 363766 の反応式
N12CCN(CC1)CC2.[NH2:9][C:10]1[N:19]=[C:18]([NH2:20])[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([S:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=3)[CH:16]=2)[N:11]=1.[OH-:30].[NH4+]>C(O)(=O)C>[NH2:9][C:10]1[N:19]=[C:18]([NH2:20])[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([S:21]([C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[C:24]([Cl:29])[CH:23]=3)=[O:30])[CH:16]=2)[N:11]=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 9237DabcoHCID 14923Ammonium HydroxideHCID 442641426-[(3,4-Dichlorophenyl)sulfanyl]quinazoline-2,4-diamine

生成物 1

HCID 125559782,4-Diamino-6-(3,4-dichlorophenylsulfinyl)quinazoline

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A suspension of 5.0 grams (0.011 mole) of the bromine complex of 1,4-diazabicyclo(2,2,2)octane in 200 mL of aqueous 70% acetic acid was stirred, and 3.4 grams (0.01 mole) of 2,4-diamino-6-(3,4-dichlorophenylthio)quinazoline was added portionwise during about a 1 hour period. Upon completion of addition, the reaction mixture was stirred at ambient temperature for about 20 hours. After this time, the reaction mixture was neutralized with concentrated ammonium hydroxide. The resultant solid was collected by filtration and triturated with methanol. The solid was collected by filtration and dried, yielding 2,4-diamino-6-(3,4-dichlorophenylsulfinyl)quinazoline, mp 200° C., dec. The NMR spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of addition
  2. stirringthe reaction mixture was stirred at ambient temperature for about 20 hours
  3. filtrationThe resultant solid was collected by filtration
  4. customtriturated with methanol
  5. filtrationThe solid was collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-ceff50bb60f646ef98b0e21ffd0bfc27
出典データセット
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05874579

反応ノート

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