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Ethyl chloroacetate → Ethyl (7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl)acetate

HRID 1699098
ノート
印刷プレビュー

反応式

HRID 1699098 の反応式
[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:13])[NH:7][C:8](=[O:12])[NH:9]2)=[CH:4][CH:3]=1.ClC1C=C2C(C(O[Si](C)(C)C)=NC(O[Si](C)(C)C)=N2)=CC=1.Cl[CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38]>C(OCC)(=O)C.CO>[Cl:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=[O:13])[NH:7][C:8](=[O:12])[N:9]2[CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])=[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

6

反応物 3

HCID 7751Ethyl chloroacetateHCID 2468587-Chloroquinazoline-2,4-diolHCID 118240197-Chloro-2,4-bis(trimethylsilyloxy)quinazoline

生成物 1

HCID 9838691Ethyl (7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl)acetate

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857
Ethyl Acetate
溶媒
2 回

実験手順

7-Chloro-2,4-dioxo-1,2,3,4-tetrahydroquinazoline (10 g) was treated as in Example 1 to give a concentrate containing 7-chloro-2,4-bis(trimethylsilyloxy)quinazoline. To this concentrate was added ethyl chloroacetate (20 ml), and the reaction was carried out at an internal temperature of 140˜150° C. for 29 hours. This reaction mixture was cooled to ≦70° C., and after addition of ethyl acetate (20 ml) , a solvent mixture of methanol (30 ml) and ethyl acetate (20 ml) was added dropwise over about 30 minutes. After completion of dropwise addition, the mixture was worked up as in Example 1 to provide ethyl 2-(7-chloro-2,4-dioxo-1,2,3,4-tetrahydroquinazolin-1-yl)acetate (13.60 g).

後処理

  1. customto give a concentrate
  2. temperatureThis reaction mixture was cooled to ≦70° C.
  3. additionwas added dropwise over about 30 minutes
  4. additionAfter completion of dropwise addition

出典と根拠

ORDレコード
ord-6ae12abef50a4670b230df58611b446c
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06344559B1

反応ノート

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