3,5-Dimethyl-4-hydroxybenzonitrile → Win 58768

HRID 4947

반응식

HRID 4947 반응식
[CH3:1][C:2]1[CH:7]=[C:6](C#N)[CH:5]=[C:4]([CH3:10])[C:3]=1[OH:11].C(C1N=NC(N2CCC(O)CC2)=CC=1)CC.CCOC(/N=N/C(OCC)=O)=O.[CH3:40][N:41]1[N:45]=[N:44][C:43]([C:46]2[CH:51]=[C:50]([CH3:52])[C:49]([OH:53])=[C:48]([CH3:54])[CH:47]=2)=[N:42]1>>[CH3:10][C:4]1[CH:5]=[C:6]([N:41]2[N:45]=[N:44][CH:43]=[N:42]2)[CH:7]=[C:2]([CH3:1])[C:3]=1[OH:11].[CH3:40][N:41]1[N:45]=[N:44][C:43]([C:46]2[CH:51]=[C:50]([CH3:52])[C:49]([OH:53])=[C:48]([CH3:54])[CH:47]=2)=[N:42]1

참가 물질

6

반응물 4

HCID 201763,5-Dimethyl-4-hydroxybenzonitrileHCID 148372Win 587682회HCID 5462977Diethyl azodicarboxylateHCID 197973046-n-Propyl-3-(4-hydroxy-1-piperidinyl)pyridazine2회

생성물 2

HCID 148372Win 58768HCID 86747187(3,5-dimethyl-4-hydroxyphenyl)-2H-tetrazole

실험 절차

2-Methyl-5-((3,5-dimethyl-4-hydroxyphenyl)-2H-tetrazole (Formula III: R2 =R3 =R4 =CH3) was prepared according to the procedure of Example 1b starting with 2,6-dimethyl-4-cyanophenol. 4.5 Mmol of 6-methyl-3-(4-hydroxyl-1-piperidinyl)pyridazine (Formula IV: R1 =methyl, Y=CH2), 1.14 g DEAD, 6.8 mmol TPP, 5 mmol of 2-methyl-5-(3,5-dimethyl-4-hydroxyphenyl)-2H-tetrazole (Formula III: R2 =R3 =R4 =CH3) were reacted as described in Example 1c. Recrystallization from ethyl acetate afforded a 71.9% yield of the compound of Formula I (R1 =R2 =R3 =R4 =methyl, Y=CH2) m.p. 183°-184° C.

후처리

  1. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-497fa056f7bb46efa7e51c283e600987
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242924

연결된 노트

불러오는 중…