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Sodium Carbonate → 4-(1-Phenylazulene-2-yl)phenylsulfonamide

HRID 1456831
ノート
印刷プレビュー

反応式

HRID 1456831 の反応式
C([NH:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[C:24]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)=[C:23]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=[CH:22]3)[C:16]=2C(OC)=O)=[CH:11][CH:10]=1)(=[O:8])=[O:7])(C)(C)C.C1(B(O)O)C=CC=CC=1.C([O-])([O-])=O.[Na+].[Na+]>C1(C)C=CC=CC=1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:25]1([C:24]2[C:23]3[C:17]([CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)=[CH:16][C:15]=2[C:12]2[CH:13]=[CH:14][C:9]([S:6]([NH2:5])(=[O:7])=[O:8])=[CH:10][CH:11]=2)[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 66827Phenylboronic AcidHCID 11145169HCID 11145169、化合物

生成物 1

HCID 221071814-(1-Phenylazulene-2-yl)phenylsulfonamide

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 1140
Toluene
溶媒

実験手順

Methyl 2- (4-t-butylaminosulfonylphenyl) -3-phenylazulene-1-carboxylate: To a solution of methyl 3-bromo-2-(4-t-butylaminosulfonylphenyl) azulene-1-carboxlate (0.56 g) in toluene (10.0 ml) was added phenylboronic acid (0.34 g), tetrakis(triphenylphosphine)palladium (0) (0.07 g) and 2M aqueous Na2CO3 (2.3 ml), and the reaction mixture was heated under reflux for 2 hr. The reaction mixture was poured into ice-water, followed by extracted with EtOAc. The combined EtOAc extracts were washed with water and brine, dried over Na2SO4, and concentrated. The crude product was purified by SiO2 column chromatography (benzenee/EtOAc, 20:1) to give the title compound (0.47 g) as violet crystals; mp 76°-77° C.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 2 hr
  3. extractionby extracted with EtOAc
  4. washThe combined EtOAc extracts were washed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customThe crude product was purified by SiO2 column chromatography (benzenee/EtOAc, 20:1)

出典と根拠

ORDレコード
ord-253ed14ad9e94e1ca4ec4e3ce1406fe8
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05843999

反応ノート

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