Water → HCID 10790583, 화합물

HRID 382337노트

반응식

HRID 382337 반응식
[Br:1]Br.[CH2:3]([C:10]1[S:14][C:13]2[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=2[C:11]=1[C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][C:28]([OH:31])=[CH:27][CH:26]=2)=[CH:21][CH:20]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C([O-])(=O)C.[K+].O>C(O)(=O)C>[CH2:3]([C:10]1[S:14][C:13]2[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=2[C:11]=1[C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:26]=[CH:27][C:28]([OH:31])=[C:29]([Br:1])[CH:30]=2)=[CH:21][CH:20]=1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24408BromineHCID 517044Potassium AcetateHCID 10548559HCID 10548559, 화합물

생성물 1

HCID 10790583HCID 10790583, 화합물수율 26.6%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

실험 절차

Bromine (1.47 mL, 28.69 mmol) in acetic acid (50 mL) was added dropwise over a 30 minutes period into a cold (5° C. mixture of 4′-(2-benzyl-benzo[b]thiophen-3-yl)-biphenyl-4-ol (7.5 g, 19.13 mmol), potassium acetate (18.6 g, 190.13 mmol), and acetic acid (200 mL). After the addition the mixture was poured into water, and extracted with ethyl ether. The organic extracts were washed with aqueous sodium bisulfite and dried over MgSO4. Evaporation and purification by flash chromatography on silica gel (hexanes/EtAOc/CH2Cl2 3:1:1) gave 4′-(2-benzyl-benzo[b]thiophen-3-yl)-3-bromo-biphenyl-4-ol as a light yellow solid (2.4 g): mp 54-56° C. MS m/e 477 (M+);

후처리

  1. additionAfter the addition the mixture
  2. extractionextracted with ethyl ether
  3. washThe organic extracts were washed with aqueous sodium bisulfite
  4. dry with materialdried over MgSO4
  5. customEvaporation and purification by flash chromatography on silica gel (hexanes/EtAOc/CH2Cl2 3:1:1)

출처 및 근거

ORD 기록
ord-7e45459e224a4c1f84317d3f133325a5
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06310081B1

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