Sodium Azide → 4-Azido-5-iodo-2-methoxybenzoic acid

HRID 1872686ノート

反応式

HRID 1872686 の反応式
[NH2:1][C:2]1[C:10]([I:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1.N([O-])=O.[Na+].[N-:18]=[N+:19]=[N-].[Na+]>FC(F)(F)C(O)=O.O>[N:1]([C:2]1[C:10]([I:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([O:12][CH3:13])[CH:3]=1)=[N+:18]=[N-:19]

参加物

6

反応物 3

HCID 33557Sodium AzideHCID 153457254-Amino-5-iodo-2-methoxybenzoic acidHCID 23668193Sodium Nitrite

生成物 1

HCID 186873664-Azido-5-iodo-2-methoxybenzoic acid収率 84.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

To a solution of 4-amino-5-iodo-2-methoxybenzoic acid (300 mg, 1.02 mmol) in trifluoroacetic acid (4 ml) at 5° C., was added sodium nitrite (283 mg, 4.1 mmol) portionwise, and the mixture allowed to stir for 30 min. Sodium azide (200 mg, 3.07 mmol) was then added portionwise and the mixture stirred for a further 30 min at 0° C. The mixture was diluted with water, and a yellow solid precipithated. The solid was filtered, washed with cold water and dried, to afford the title compound (274 mg, 84%).

後処理

  1. stirringthe mixture stirred for a further 30 min at 0° C
  2. filtrationThe solid was filtered
  3. washwashed with cold water
  4. customdried

出典と根拠

ORDレコード
ord-c73db79b26e746e5918b2a329a71343b
出典データセット
uspto-grants-2000_08
特許番号
US06110934

反応ノート

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