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Ammonia → 1,3-Dichloro-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazoline hydrochloride (1:1)

HRID 375611
ノート
印刷プレビュー

反応式

HRID 375611 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]([Cl:12])[CH:9]=[C:8]2[C:3]=1[C:4](=O)[N:5]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][C:6]1=[N:7]2.C(Cl)(Cl)Cl.CO.N>C([SiH](CC)CC)C.[Cl-].[Zn+2].[Cl-]>[ClH:1].[Cl:1][C:2]1[CH:11]=[C:10]([Cl:12])[CH:9]=[C:8]2[C:3]=1[CH2:4][N:5]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][C:6]1=[N:7]2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 222AmmoniaHCID 887MethanolHCID 6212ChloroformHCID 10039448HCID 10039448、化合物

生成物 1

HCID 189922831,3-Dichloro-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazoline hydrochloride (1:1)

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒
HCID 12052
Triethylsilane
溶媒
3 回

実験手順

To a solution of 1 g of 1,3-dichloro-7,8,9,10-tetrahydroazepino[2,1-b]quinazolin-12(6H)-one in 15 mL of triethylsilane was added 8 g of anhydrous zinc chloride and the mixture was refluxed under nitrogen with vigorous stirring. The triethylsilane was replenished in about 8-hour intervals. When the reaction was judged complete by TLC (300:25:1 chloroform:methanol: 28% aqueous ammonia, basified aliquot) the excess of triethylsilane and other volatiles were removed in vacuo and the residue was purified and worked-up as in Method A to give the desired 1,3-dichloro-6,7,8,9,10,12-hexahydroazepino[2,1-b]quinazoline hydrochloride as white crystalline solid.

後処理

  1. temperaturethe mixture was refluxed under nitrogen with vigorous stirring
  2. customwere removed in vacuo
  3. customthe residue was purified and worked-up as in Method A

出典と根拠

ORDレコード
ord-7c94258826554197ba66b102f8e23eb6
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05486512

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