Triethylamine → HCID 178509964、化合物

HRID 626706ノート

反応式

HRID 626706 の反応式
[N:1]([C:4]1[C:9]([Cl:10])=[CH:8][N:7]=[CH:6][C:5]=1[CH:11]=O)=[N+:2]=[N-:3].[NH2:13][C:14]1[C:21]([Cl:22])=[CH:20][C:17]([C:18]#[N:19])=[CH:16][C:15]=1[Cl:23].C(N(CC)CC)C>C(Cl)Cl.[Ti](Cl)(Cl)(Cl)Cl>[N:1]([C:4]1[C:9]([Cl:10])=[CH:8][N:7]=[CH:6][C:5]=1/[CH:11]=[N:13]/[C:14]1[C:15]([Cl:23])=[CH:16][C:17]([C:18]#[N:19])=[CH:20][C:21]=1[Cl:22])=[N+:2]=[N-:3]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 5227064-Amino-3,5-dichlorobenzonitrileHCID 866970494-Azido-5-chloropyridine-3-carbaldehyde

生成物 1

HCID 178509964HCID 178509964、化合物

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

実験手順

To a cooled (0° C.) solution of 4-azido-5-chloropyridine-3-carbaldehyde (2.0 g, 10.95 mmol), 4-amino-3,5-dichlorobenzonitrile (2.05 g, 10.95 mmol) and triethylamine (4.6 mL, 6.57 mmol) in DCM (48 mL) was added titanium tetrachloride (1M in DCM, 6.6 mL, 6.57 mmol) dropwise over 10 minutes. The reaction mixture was stirred for 20 minutes, warmed to room temperature, and stirred for an additional 30 minutes. The resultant mixture was concentrated to dryness under reduced pressure to afford the title compound which was used without further purification.

後処理

  1. stirringstirred for an additional 30 minutes
  2. concentrationThe resultant mixture was concentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-13808bc4382147c0974a175fb83b2414
出典データセット
uspto-grants-2016_04
特許番号
US09309240B2

反応ノート

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