Water → HCID 178497602、化合物

HRID 337378

反応式

HRID 337378 の反応式
[C:1]([C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][CH:4]=1)#[N:2].Cl.C(N(CC)CC)C.[N-:21]=[N+:22]=[N-:23].[Na+].O>C1(C)C=CC=CC=1>[NH:21]1[C:1]([C:3]2[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][CH:4]=2)=[N:2][N:23]=[N:22]1

参加物

6

反応物 4

HCID 962WaterHCID 11130Triethylamine hydrochlorideHCID 33557Sodium AzideHCID 70791Methyl 4-cyanobenzoate

生成物 1

HCID 178497602HCID 178497602、化合物収率 96%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.16 g (10 mmol) of methyl 4-cyanobenzoate, 2.06 g (15 mmol) of triethylamine hydrochloride and 0.98 g (15 mmol) of sodium azide in toluene (20 ml) was allowed to react at 100° C. for 16 hours, and after cooling to room temperature, water (20 ml) was added, and the reaction solution was allowed to separate. Concentrated hydrochloric acid was added to the aqueous layer, and the precipitated colorless solid was collected by filtration through a Kiriyama funnel and dried under reduced pressure to obtain methyl 4-(1H-tetrazol-5-yl)benzoate (1.96 g, yield 96%).

後処理

  1. customto react at 100° C. for 16 hours
  2. customto separate
  3. additionConcentrated hydrochloric acid was added to the aqueous layer
  4. filtrationthe precipitated colorless solid was collected by filtration through a Kiriyama funnel
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-22dbf1ff3bc84e5ea39efa4f046eef76
出典データセット
uspto-grants-2014_11
特許番号
US08889732B2

関連ノート

読み込み中…