Hydrochloric Acid → HCID 69669367, 화합물

HRID 929999노트

반응식

HRID 929999 반응식
[C:1]1([C:14]2[CH:15]=[C:16](Br)[CH:17]=[C:18]([C:20]3[C:32]4[NH:31][C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[C:24]=4[CH:23]=[CH:22][CH:21]=3)[CH:19]=2)[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.C([Li])CCC.[B:39](OC)([O:42]C)[O:40]C.Cl>O1CCCC1>[C:1]1([C:14]2[CH:15]=[C:16]([B:39]([OH:42])[OH:40])[CH:17]=[C:18]([C:20]3[C:32]4[NH:31][C:30]5[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=5)[C:24]=4[CH:23]=[CH:22][CH:21]=3)[CH:19]=2)[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8470Trimethyl borateHCID 23089769HCID 23089769, 화합물HCID 178418339Butyllithium

생성물 1

HCID 69669367HCID 69669367, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Under an Ar atmosphere, 3,5-dicarbazolylbromobenzene (4.87 g, 0.01 mol) and 100 mL THF (tetrahydrofuran) were added into a 250 mL single-necked flask, then 9.4 mL n-BuLi (n-butyllithium) (1.6 M n-hexane solution) was added, stirred and reacted at −78° C. for 1.5 h. After this, trimethyl borate was added and reacted for 12 h, and then 20 mL hydrochloric acid solution was added, acidified for 0.5 h. After the reaction was completed, we carried out liquid separation, drying, and concentrating under reduced pressure, and obtained 3,5-dicarbazolylphenylboronic acid by column chromatography. The reaction process is as follows:

후처리

  1. customreacted at −78° C. for 1.5 h
  2. customreacted for 12 h
  3. customliquid separation
  4. customdrying
  5. concentrationconcentrating under reduced pressure

출처 및 근거

ORD 기록
ord-e1131bb6cc6340f4a58e07cb57e9e637
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09296738B2

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