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Diethyl Ether → 5-[(1E)-3-azidobut-1-enyl]-2-(4-isopropoxyphenoxy)-1,3-thiazole

HRID 2078453
ノート
印刷プレビュー

反応式

HRID 2078453 の反応式
C(O[CH:5]([CH3:24])/[CH:6]=[CH:7]/[C:8]1[S:12][C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH:21]([CH3:23])[CH3:22])=[CH:16][CH:15]=2)=[N:10][CH:9]=1)(=O)C.[N-:25]=[N+:26]=[N-:27].[Na+].CCOCC.CCCCCC>O1CCCC1.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>[N:25]([CH:5]([CH3:24])/[CH:6]=[CH:7]/[C:8]1[S:12][C:11]([O:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH:21]([CH3:23])[CH3:22])=[CH:16][CH:15]=2)=[N:10][CH:9]=1)=[N+:26]=[N-:27]
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 4

HCID 3283Diethyl EtherHCID 8058HexaneHCID 33557Sodium Azide3 回HCID 67096975(2E)-3-[2-(4-isopropoxyphenoxy)-1,3-thiazol-5-yl]-1-methylprop-2-enyl acetate

生成物 1

HCID 866212085-[(1E)-3-azidobut-1-enyl]-2-(4-isopropoxyphenoxy)-1,3-thiazole収率 57.6%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

To a solution of the product of Example 7E (155 mg, 0.45 mmole) in tetrahydrofuran (15 mL) was added sodium azide (32 mg, 0.5 mmole) and tetrakis(triphenylphosphine)palladium(0) (25 mg, 0.022 mmole) and heated at 50° C. After 2 hours additional sodium azide (23 mg, 0.35 mmole) was added and after 8 hours a third amount of sodium azide (40 mg, 0.61 mmole) was added and stirred at 50° C. overnight. The reaction mixture was added ether and hexane and the organic phase was washed twice with water followed by brine. The reaction mixture was dried over magnesium sulfate filtered and evaporated. The product was purified via silica column, using a gradient of 5-25% ethyl acetate in hexane and yielded 85 mg (57.6%) of clear oil. 1H NMR (300 MHz, CDCl3) δ ppm 7.13-7.22 (m, 2H) 7.10 (s, 1H) 6.86-6.98 (m, 2H) 6.58 (d, J=15.44 Hz, 1H) 5.69 (dd, J=15.63, 7.17 Hz, 1H) 4.42-4.62 (m, 1H) 3.96-4.23 (m, 1H) 1.35 (d, J=5.88 Hz, 6H) 1.33 (d, J=5.88 Hz, 3H). Mass spectrum DCI 331 (M+H)+.

後処理

  1. additionwas added
  2. washthe organic phase was washed twice with water
  3. dry with materialThe reaction mixture was dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe product was purified via silica column

出典と根拠

ORDレコード
ord-34725e1695e94e9e96083f0589fdc7be
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928243B2

反応ノート

読み込み中…

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