Water → HCID 14517625、化合物

HRID 1073675ノート

反応式

HRID 1073675 の反応式
[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:22])=[CH:13][C:14]3[O:19][CH2:18][C:17](=[O:20])[NH:16][C:15]=3[CH:21]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2.[H-].[Na+].[CH2:25](I)[CH3:26].O>CN(C)C=O>[Cl:1][C:2]1[N:3]([C:11]2[C:12]([F:22])=[CH:13][C:14]3[O:19][CH2:18][C:17](=[O:20])[N:16]([CH2:25][CH3:26])[C:15]=3[CH:21]=2)[N:4]=[C:5]2[C:10]=1[CH2:9][CH2:8][CH2:7][CH2:6]2

参加物

6

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 24758Sodium hydrideHCID 14517660HCID 14517660、化合物

生成物 1

HCID 14517625HCID 14517625、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-chloro-2-[7-fluoro-2H-1,4- benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-indazole (1.0 g) in N,N-dimethylformamide (10 ml), sodium hydride (0.3 g) and ethyl iodide (0.5 g) were successively added, and the resultant mixture was heated at 50° to 60° C., followed by stirring for 3 hours. The reaction mixture was poured into water, and the precipitated crystals were collected by filtration and purified by silica gel column chromatography using a mixture of ethyl acetate and hexane as an eluent to give Compound No. 1 (0.9 g). m.p., 101.5°-102.5° C.

後処理

  1. filtrationthe precipitated crystals were collected by filtration
  2. custompurified by silica gel column chromatography
  3. additiona mixture of ethyl acetate and hexane as an eluent
  4. customto give Compound No
  5. customm.p., 101.5°-102.5° C.

出典と根拠

ORDレコード
ord-24b93337d381418abac861c50bbd8ed4
出典データセット
uspto-grants-1990_11
特許番号
US04970322

反応ノート

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