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

HRID 1699096노트

반응식

HRID 1699096 반응식
[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].Br[Si](C)(C)C>C1(=O)OC(C)CO1>[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

참가 물질

6

반응물 4

HCID 7751Ethyl chloroacetateHCID 76113BromotrimethylsilaneHCID 2468587-Chloroquinazoline-2,4-diolHCID 118240197-Chloro-2,4-bis(trimethylsilyloxy)quinazoline

생성물 1

HCID 9838691Ethyl (7-chloro-2,4-dioxo-3,4-dihydroquinazolin-1(2H)-yl)acetate수율 97%

시약·촉매·용매 1

HCID 7924Propylene Carbonate용매

실험 절차

As in Example 1, 7-chloro-2,4-dioxo-1,2,3,4-tetrahydroquinazoline (20 g) was silylated and the toluene was distilled off to give a concentrate containing 7-chloro-2,4-bis(trimethylsilyloxy)quinazoline. To this concentrate were added propylene carbonate (40 ml), ethyl chloroacetate (16.21 g) and bromotrimethylsilane (3.11 g), and the reaction was carried out at an internal temperature of 125˜140° C. for 8 hours. This reaction mixture was cooled to ≦70° C. and worked up as in Example 1 to provide ethyl 2-(7-chloro-2,4-dioxo-1,2,3,4-tetrahydroquinazolin-1-yl)acetate (27.90 g).

후처리

  1. distillationthe toluene was distilled off
  2. customto give a concentrate
  3. temperatureThis reaction mixture was cooled to ≦70° C.

출처 및 근거

ORD 기록
ord-caae2dbec16b4071988a39a56fb4d73a
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06344559B1

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