Triethylamine → HCID 178509964, 화합물

HRID 626706노트

반응식

HRID 626706 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 178509964HCID 178509964, 화합물

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-13808bc4382147c0974a175fb83b2414
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309240B2

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