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

HRID 1872686노트

반응식

HRID 1872686 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 186873664-Azido-5-iodo-2-methoxybenzoic acid수율 84.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6422Trifluoroacetic acid용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-c73db79b26e746e5918b2a329a71343b
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06110934

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