Isopropylamine → HCID 18446929、化合物

HRID 1983072ノート

反応式

HRID 1983072 の反応式
[CH:1]([NH2:4])([CH3:3])[CH3:2].[Cl:5][C:6]1[C:7]([N:12]2[C:16]([C:17]3[O:22][C:21](=[O:23])[C:20]4[CH:24]=[C:25]([N+:29]([O-:31])=[O:30])[CH:26]=[C:27]([CH3:28])[C:19]=4[N:18]=3)=[CH:15][C:14]([C:32]([F:35])([F:34])[F:33])=[N:13]2)=[N:8][CH:9]=[CH:10][CH:11]=1>O1CCOCC1>[Cl:5][C:6]1[C:7]([N:12]2[C:16]([C:17]([NH:18][C:19]3[C:20]([C:21]([NH:4][CH:1]([CH3:3])[CH3:2])=[O:23])=[CH:24][C:25]([N+:29]([O-:31])=[O:30])=[CH:26][C:27]=3[CH3:28])=[O:22])=[CH:15][C:14]([C:32]([F:35])([F:34])[F:33])=[N:13]2)=[N:8][CH:9]=[CH:10][CH:11]=1

参加物

4

反応物 2

HCID 6363IsopropylamineHCID 690644832-[1-(3-Chloro-2-pyridinyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl]-8-methyl-6-nitro-4H-3,1-benzoxazin-4-one

生成物 1

HCID 18446929HCID 18446929、化合物収率 14.3%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

Isopropyl amine (0.35 mL, 4.11 mmol) was added to a solution of 619 mg (1.37 mmol) of the product of Step B in dioxane (8 mL) at 25° C. After being stirred overnight, the resulting heterogenous mixture was concentrated and the residue was triturated with methanol (10 mL). Filtration gave 100 mg of the title product. The filtrate was concentrated and the resulting residue was triturated with diethyl ether. Filtration of the resulting solid provided an additional 320 mg of the title product, m.p. 170-172° C.

後処理

  1. concentrationthe resulting heterogenous mixture was concentrated
  2. customthe residue was triturated with methanol (10 mL)
  3. filtrationFiltration

出典と根拠

ORDレコード
ord-884240302a6a4e819bbe11983f6cd039
出典データセット
uspto-grants-2009_06
特許番号
US07541377B2

反応ノート

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