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Toluene → HCID 178504566、化合物

HRID 2275240
ノート
印刷プレビュー

反応式

HRID 2275240 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:12](=[CH:13][C:14]=1[Cl:15])[NH:11][C:10]1[C:9]([CH3:17])([CH3:16])[C:8]3[CH:18]=[C:19]([OH:22])[CH:20]=[CH:21][C:7]=3[C:6](=[O:23])[C:5]2=1.[Si:24]([O:31][CH2:32][C@H:33]1[O:37][C:36]([CH3:39])([CH3:38])[O:35][C@@H:34]1O)([C:27](C)(C)C)([CH3:26])C.[C:41]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:60]1([CH3:66])[CH:65]=CC=C[CH:61]=1.CCOC(/N=N/C(OCC)=O)=O>C1COCC1>[C:60]([C@@H:32]([O:31][SiH:24]([CH3:26])[CH3:27])[C@@H:33]1[O:37][C:36]([CH3:38])([CH3:39])[O:35][CH:34]1[CH2:41][O:22][C:19]1[CH:20]=[CH:21][C:7]2[C:6](=[O:23])[C:5]3[C:4]4[C:12](=[CH:13][C:14]([Cl:15])=[C:2]([Cl:1])[CH:3]=4)[NH:11][C:10]=3[C:9]([CH3:17])([CH3:16])[C:8]=2[CH:18]=1)([CH3:66])([CH3:65])[CH3:61]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 1140TolueneHCID 11776TriphenylphosphineHCID 5462977Diethyl azodicarboxylateHCID 66834506(4S,5R)-5-(tert-butyldimethylsilanyloxymethyl)-2,2-dimethyl-[1,3]dioxolan-4-olHCID 668345622,3-Dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one

生成物 1

HCID 178504566
HCID 178504566、化合物
収率 67%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

Under nitrogen atmosphere, to the THF (0.3 mL) solution of 2,3-dichloro-8-hydroxy-6,6-dimethyl-5,6-dihydro-benzo[b]carbazol-11-one (Compound Y4, 12.9 mg, 0.0373 mmol), (4S,5R)-5-(tert-butyldimethylsilanyloxymethyl)-2,2-dimethyl-[1,3]dioxolan-4-ol (15.5 mg, 0.0559 mmol) and triphenylphosphine (14.7 mg, 0.0559 mmol), toluene solution (25.4 μL, 0.0559 mmol) of DEAD was added dropwise at room temperature. The reaction mixture was stirred at ambient temperature of 40° C. for 4 hr. After cooling to room temperature, the reaction mixture was concentrated under reduced pressure, and the resulting crude product was purified by preparative TLC (Merck 60 F254, 0.5 mm) {solution for elution:hexane/ethyl acetate (3:1)} to obtain the title compound (white solid, 15.1 mg, 67%).

後処理

  1. temperatureAfter cooling to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customthe resulting crude product was purified by preparative TLC (Merck 60 F254, 0.5 mm)
  4. washfor elution

出典と根拠

ORDレコード
ord-2cf8f5676f7e4b88a6241abe7e1f2244
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09126931B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート