2,6-Difluorobenzoyl chloride → HCID 9860931、化合物

HRID 567683

反応式

HRID 567683 の反応式
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[F:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:15]=1[C:16](Cl)=O.C(NC1C=CC2N=C(C3C(F)=CC=CC=3F)OC(=O)C=2C=1)(=O)C>C(N(CC)CC)C.C1(C)C=CC=CC=1>[F:13][C:14]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:15]=1[C:16]1[O:5][C:4](=[O:6])[C:3]2[CH:7]=[C:8]([F:12])[C:9]([F:11])=[CH:10][C:2]=2[N:1]=1

参加物

5

反応物 3

HCID 874382,6-Difluorobenzoyl chlorideHCID 7359652-Amino-4,5-difluorobenzoic acidHCID 99488136-Acetamido-(2,6-difluoro-phenyl)-benzo[d][1,3]oxazin-4-one

生成物 1

HCID 9860931HCID 9860931、化合物

試薬・触媒・溶媒 1

HCID 22504574Toluene triethylamine溶媒

実験手順

2-Amino-4,5-difluorobenzoic acid (0.5 g), 2,6-difluorobenzoyl chloride (0.80 mL) and triethyl amine/toluene (1/1) (18 mL) were reacted as described under (10). Reaction time 1 day. Extraction between ethyl acetate (20 mL) and HCl (2N,20 mL), followed by separation of the organic toluene and precipitated with hexane. The resulting mixture was further purified on a silicagel column using dichloromethane as eluent. The isolated fraction identified as 2-(2,6-difluoro-phenyl)-6,7-difluoro-benzo[d][1,3]oxazin-4-one (0.71 g), mp. 165 C, MS m/e: 295 M+.

後処理

  1. customReaction time 1 day
  2. extractionExtraction between ethyl acetate (20 mL) and HCl (2N,20 mL)
  3. customfollowed by separation of the organic toluene
  4. customprecipitated with hexane
  5. customThe resulting mixture was further purified on a silicagel column

出典と根拠

ORDレコード
ord-a2fa7b48033c463e94febb15bcd28172
出典データセット
uspto-grants-2001_01
特許番号
US06180625B2

関連ノート

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