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Hydrochloric Acid → HCID 68452746、化合物

HRID 2357649
ノート
印刷プレビュー

反応式

HRID 2357649 の反応式
[C:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]=[C:15]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:16](OC)=[O:17])=[CH:10][CH:11]=2)[CH:6]=[N:5][N:4]=1)#[N:2].Cl.[CH:25]1([NH2:28])[CH2:27][CH2:26]1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>C(OCC)(=O)C.CN(C=O)C>[C:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]3[CH:14]=[C:15]([CH:20]=[CH:21][C:22]=3[CH3:23])[C:16]([NH:28][CH:25]3[CH2:27][CH2:26]3)=[O:17])=[CH:10][CH:11]=2)[CH:6]=[N:5][N:4]=1)#[N:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 69828CyclopropylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 68455479HCID 68455479、化合物

生成物 1

HCID 68452746HCID 68452746、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
120 °C

実験手順

To methyl 3-(1-cyanophthalazin-6-yl)-4-methylbenzoate (0.800 g, 2.6 mmol) was added 6N HCl (10.6 mL) and the reaction was heated in a microwave oven for 25 min at 120° C. The reaction was concentrated, dried in vacuo and DMF (5.3 mL) and cyclopropylamine (0.92 mL, 13 mmol) were added. HATU (2.0 g, 5.3 mmol) was added and the reaction mixture was stirred at RT for 1 h, then diluted with 75 mL ethyl acetate, partitioned with sodium bicarbonate (saturated, aqueous), and the organic layers were washed 2×20 mL with sodium bicarbonate (saturated, aqueous), separated, dried over sodium sulfate, concentrated in vacuo, and purified by HPLC to give the title compound. MS (ES+): 329(M+H)+.

後処理

  1. concentrationThe reaction was concentrated
  2. additionwere added
  3. custompartitioned with sodium bicarbonate (saturated, aqueous)
  4. washthe organic layers were washed 2×20 mL with sodium bicarbonate (saturated, aqueous)
  5. customseparated
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated in vacuo
  8. custompurified by HPLC

出典と根拠

ORDレコード
ord-15ac612c413d4d75886c89582ee75fdc
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759337B2

反応ノート

読み込み中…

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