Triethylamine → 3-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]-N-tricyclo[3.3.1.13,7]dec-1-ylpropanamide

HRID 5495

반응식

HRID 5495 반응식
[CH3:1][C:2]([C:5]1[CH:10]=[C:9]([SH:11])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:4])[CH3:3].[C:17]12([NH:27][C:28](=[O:31])[CH:29]=[CH2:30])[CH2:26][CH:21]3[CH2:22][CH:23]([CH2:25][CH:19]([CH2:20]3)[CH2:18]1)[CH2:24]2.C(N(CC)CC)C>CO>[CH3:4][C:2]([C:5]1[CH:10]=[C:9]([S:11][CH2:30][CH2:29][C:28]([NH:27][C:17]23[CH2:24][CH:23]4[CH2:22][CH:21]([CH2:20][CH:19]([CH2:25]4)[CH2:18]2)[CH2:26]3)=[O:31])[CH:8]=[C:7]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:6]=1[OH:16])([CH3:1])[CH3:3]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 703702,6-Di-tert-butyl-4-mercaptophenolHCID 284637N-(Adamantan-1-yl)prop-2-enimidic acid

생성물 1

HCID 149865643-[[3,5-bis(1,1-dimethylethyl)-4-hydroxyphenyl]thio]-N-tricyclo[3.3.1.13,7]dec-1-ylpropanamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Following the method of Example 4, 2,6-bis(1,1-dimethylethyl)-4-mercaptophenol (1.19 g, 0.005 mole), the title compound of Example 5 (1.03 g, 0.005 mole) and triethylamine (0.5 ml) were stirred in methanol (100 ml) for 12 hours at room temperature under argon. The solvent and triethylamine were removed on a rotary evaporator and the product purified by chromatography on silica, recrystallized from ethyl aceate/hexane, filtered and dried in vacuo, m.p. ca.172.5°-173.5° C.

후처리

  1. customThe solvent and triethylamine were removed on a rotary evaporator
  2. customthe product purified by chromatography on silica
  3. customrecrystallized from ethyl aceate/hexane
  4. filtrationfiltered
  5. customdried in vacuo, m.p. ca
  6. custom172.5°-173.5° C.

출처 및 근거

ORD 기록
ord-390ae00531e84ce6ba81f1cd2e927cdd
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05244899

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