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

HRID 648752
ノート
印刷プレビュー

反応式

HRID 648752 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-a1d5b033f12541b5bba441529185d808
出典データセット
uspto-grants-1988_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04736033

反応ノート

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