Triethyl orthoacetate → 2-Methyl-6-nitro-1,3-benzoxazol-4-ol

HRID 647221노트

반응식

HRID 647221 반응식
[NH2:1][C:2]1[C:8]([OH:9])=[CH:7][C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:3]=1[OH:4].[C:13](OCC)(OCC)(OCC)[CH3:14]>C1(C)C=CC=CC=1.C1COCC1>[N+:10]([C:6]1[CH:5]=[C:3]([OH:4])[C:2]2[N:1]=[C:13]([CH3:14])[O:9][C:8]=2[CH:7]=1)([O-:12])=[O:11]

참가 물질

5

반응물 2

HCID 66221Triethyl orthoacetateHCID 204858732-Amino-5-nitrobenzene-1,3-diol

생성물 1

HCID 204858692-Methyl-6-nitro-1,3-benzoxazol-4-ol수율 39.4%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of the 2-amino-5-nitroresorcinol (2.9 g, 0.017 mole) in toluene (50 ml) and THF (5 ml) was added triethyl orthoacetate (4.1 g, 0.0255 mole). This mixture was heated to reflux for one hour. Upon cooling, the product crystallized out of solution and was collected and dried to yield a tan solid (1.3 g, 39.4 percent). TLC showed the product to be pure.

후처리

  1. temperatureThis mixture was heated
  2. temperatureto reflux for one hour
  3. temperatureUpon cooling
  4. customthe product crystallized out of solution
  5. customwas collected
  6. customdried

출처 및 근거

ORD 기록
ord-96063322e09144ec92f8a70e1a7ff405
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04407930

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