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Triethylamine → HCID 59255329、化合物

HRID 78270
ノート
印刷プレビュー

反応式

HRID 78270 の反応式
[C:1]([C:3]1[C:4]([NH2:10])=[N:5][C:6]([NH2:9])=[CH:7][CH:8]=1)#[CH:2].[F:11][C:12]1[CH:28]=[CH:27][C:15]([CH2:16][C:17]2[O:21][C:20]([CH2:22][C:23](Cl)=[N:24][OH:25])=[CH:19][CH:18]=2)=[CH:14][CH:13]=1.C(N(CC)CC)C>O1CCCC1>[F:11][C:12]1[CH:28]=[CH:27][C:15]([CH2:16][C:17]2[O:21][C:20]([CH2:22][C:23]3[CH:2]=[C:1]([C:3]4[C:4]([NH2:10])=[N:5][C:6]([NH2:9])=[CH:7][CH:8]=4)[O:25][N:24]=3)=[CH:19][CH:18]=2)=[CH:14][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 552816763-Ethynylpyridine-2,6-diamineHCID 72262865(5-(4-Fluorobenzyl)-furan-2-yl)acetohydroximoyl chloride

生成物 1

HCID 59255329HCID 59255329、化合物収率 33%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a tetrahydrofuran (3 mL) solution of 3-ethynyl-pyridin-2,6-diamine (50 mg, 0.376 mmol) described in Manufacturing Example 13-1-3 and (5-(4-fluorobenzyl)-furan-2-yl)acetohydroximoyl chloride (161 mg, 0.602 mmol) described in Manufacturing Example 208-1-5 was added triethylamine (131 μL, 0.94 mmol), which was stirred for 19 hours at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=1:1, then ethyl acetate) to obtain the title compound (45 mg, 33%).

後処理

  1. customThis mixture was partitioned into ethyl acetate and water
  2. customThe organic layer was separated
  3. washwashed with water and saturated aqueous sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under a reduced pressure
  7. customthe residue was purified by NH silica gel column chromatography (ethyl acetate

出典と根拠

ORDレコード
ord-8b790e6580264ba4aa6238fd0a91fa97
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841327B2

反応ノート

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