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Hydrochloric Acid → 2-Amino-5,6,7,8-tetrahydroquinazolin-6-one

HRID 34657
ノート
印刷プレビュー

反応式

HRID 34657 の反応式
[CH3:1][N:2]([CH:4]([N:8](C)C)[N:5](C)[CH3:6])C.C1(=O)[CH2:16][CH2:15][C:14](=[O:17])[CH2:13][CH2:12]1.C(=O)(O)O.NC(N)=N.Cl>C1(C)C=CC=CC=1.CO>[O:17]=[C:14]1[CH2:15][CH2:16][C:6]2[N:5]=[C:4]([NH2:8])[N:2]=[CH:1][C:12]=2[CH2:13]1
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 313Hydrochloric AcidHCID 125111,4-CyclohexanedioneHCID 79831N,N,N',N',N'',N''-HexamethylmethanetriamineHCID 286947Carbonic acid-guanidine (1:1)

生成物 1

HCID 212982302-Amino-5,6,7,8-tetrahydroquinazolin-6-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 1140
Toluene
溶媒
2 回

実験手順

A solution of tris(dimethylamino)methane, 25.0 g (172 mmol), in 100 ml toluene is added dropwise, under nitrogen, to a solution of the monoethylene ketal of 1,4-cyclohexanedione, 25.0 g (160 mmol), in 300 ml of toluene. The resulting solution is evaporated in-vacuo and the residue is dissolved in 600 ml of methanol along with 38.72 g (320 mmol) of guanidine carbonate. The pH of the solution is adjusted to 9 with 15% hydrochloric acid and the mixture is refluxed for 16 hours. The solvent is evaporated and the yellow residue is washed with cold water and recrystallized from absolute ethanol to yield 11.0 g of 5,6,7,8-tetrahydro-6-ketoquinazolin-2-amine, ethylene ketal as yellow prisms; mp 214°-217° C.

後処理

  1. customThe resulting solution is evaporated in-vacuo
  2. temperaturethe mixture is refluxed for 16 hours
  3. customThe solvent is evaporated
  4. washthe yellow residue is washed with cold water
  5. customrecrystallized from absolute ethanol

出典と根拠

ORDレコード
ord-999f0d60f88a46828744633fb78cedb5
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04762843

反応ノート

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