Triethylamine hydrochloride → HCID 178506136、化合物

HRID 1924428ノート

反応式

HRID 1924428 の反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[C:5]#[N:6].[N-:13]=[N+:14]=[N-:15].[Na+].Cl.C(N(CC)CC)C>C1(C)C=CC=CC=1>[F:1][C:2]([F:11])([F:12])[C:3]1[CH:10]=[CH:9][CH:8]=[CH:7][C:4]=1[C:5]1[NH:15][N:14]=[N:13][N:6]=1

参加物

5

反応物 3

HCID 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 679722-(Trifluoromethyl)benzonitrile

生成物 1

HCID 178506136HCID 178506136、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
110 °C

実験手順

A vigorously stirred suspension of 2-(trifluoromethyl)benzonitrile (2-A) (6.34 g, 37 mmol), sodium azide (4.81 g, 74 mmol) and triethylamine hydrochloride (10.19 g, 74 mmol) in toluene (70 mL) was heated at 110° C. for 48 h. The mixture was cooled and extracted twice with water. The combined extracts were washed with hexane and brought to pH about 1 with concentrated HCl. The precipitate which formed was filtered, washed with water and dried to give 5-[2-(trifluoromethyl)phenyl]-1H-tetrazole (2-B).

後処理

  1. temperatureThe mixture was cooled
  2. extractionextracted twice with water
  3. washThe combined extracts were washed with hexane
  4. customThe precipitate which formed
  5. filtrationwas filtered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-d4a4c10ce4dc490b844a1ab037243215
出典データセット
uspto-grants-2012_05
特許番号
US08178546B2

反応ノート

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