Hydrochloric Acid → HCID 69669367、化合物

HRID 929999ノート

反応式

HRID 929999 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8470Trimethyl borateHCID 23089769HCID 23089769、化合物HCID 178418339Butyllithium

生成物 1

HCID 69669367HCID 69669367、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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:

後処理

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

出典と根拠

ORDレコード
ord-e1131bb6cc6340f4a58e07cb57e9e637
出典データセット
uspto-grants-2016_03
特許番号
US09296738B2

反応ノート

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