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2-Chlorobutanoyl chloride → 4H-3,1-Benzoxazin-4-one, 2-(1-chloropropyl)-8-(trifluoromethyl)-

HRID 648752
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반응식

HRID 648752 반응식
[Cl:1][CH:2]([CH2:6][CH3:7])[C:3](Cl)=[O:4].[NH2:8][C:9]1[C:17]([C:18]([F:21])([F:20])[F:19])=[CH:16][CH:15]=[CH:14][C:10]=1[C:11](O)=[O:12]>C1(C)C=CC=CC=1>[Cl:1][CH:2]([C:3]1[O:4][C:11](=[O:12])[C:10]2[CH:14]=[CH:15][CH:16]=[C:17]([C:18]([F:19])([F:20])[F:21])[C:9]=2[N:8]=1)[CH2:6][CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1390532-Chlorobutanoyl chlorideHCID 6045692-Amino-3-(trifluoromethyl)benzoic acid

생성물 1

HCID 134230814H-3,1-Benzoxazin-4-one, 2-(1-chloropropyl)-8-(trifluoromethyl)-수율 97.2%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A suspension of 20.3 g of 2-chloro-butyryl chloride and 12.3 g of 2-amino-3-trifluoromethyl-benzoic acid in toluene was refluxed under reduced pressure for one hour and was then evaporated to dryness under reduced pressure. The oil residue was added to 100 ml of iced water and the mixture was stirred for one hour and was vacuum filtered. The product was washed with water and dried under reduced pressure at 50° C. to obtain 17 g of 2-(1-chloropropyl)-8-trifluoromethyl-4H-3,1-benzoxazine-4-one melting at 65°-70° C.

후처리

  1. temperaturewas refluxed under reduced pressure for one hour
  2. customwas then evaporated to dryness under reduced pressure
  3. additionThe oil residue was added to 100 ml of iced water
  4. filtrationfiltered
  5. washThe product was washed with water
  6. customdried under reduced pressure at 50° C.

출처 및 근거

ORD 기록
ord-a1d5b033f12541b5bba441529185d808
출처 데이터셋
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04736033

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