Diethylenetriamine → 2-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazole

HRID 1197634

반응식

HRID 1197634 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[N:10]=[N:11][C:12]1[CH:17]=[C:16]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:15]=[C:14]([C:22]([CH3:25])([CH3:24])[CH3:23])[C:13]=1[OH:26])([O-])=O.NCCNCCN>C1(C)C(C)=CC=CC=1>[OH:26][C:13]1[C:14]([C:22]([CH3:25])([CH3:24])[CH3:23])=[CH:15][C:16]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:17][C:12]=1[N:11]1[N:10]=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]2=[N:1]1

참가 물질

4

반응물 2

HCID 8111Diethylenetriamine2회HCID 1041102,4-Bis(1,1-dimethylethyl)-6-[2-(2-nitrophenyl)diazenyl]phenol

생성물 1

HCID 774552-(2'-Hydroxy-3'5-di-tert-butylphenyl) benzotriazole수율 90%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Example 1 is repeated, except that an equivalent amount of 2-nitro-2'-hydroxy-3', 5'-di-tert.-butylazobenzene (91% pure) is used instead of 2-nitro-2'-hydroxy-5'-methylazobenzene and a mixture of 40 g of xylene and 60 g of diethylenetriamine instead of 80 g of xylene and 20 g of diethylenetriamine. The hydrogenation is carried out at 50° C. After work up of the hydrogenation solution, the product is crystallized from a mixture of 40 g of xylene and 160 g of methanol. The product (title compound) is isolated in a yield of 90% of theory. Melting point: 152°-154° C.

후처리

  1. customis carried out at 50° C
  2. customAfter work up of the hydrogenation solution, the product is crystallized from a mixture of 40 g of xylene and 160 g of methanol

출처 및 근거

ORD 기록
ord-023e4e77b12242cca474cc7c639b7fb3
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05276161

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