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Sodium Carbonate → (2-Chloro-4-naphthalen-1-yl-phenyl)-(10,11-dihydro-5H-pyrrolo[2,1-c][1,4] benzodiazepin-10-yl)-methanone

HRID 1830068
ノート
印刷プレビュー

反応式

HRID 1830068 の反応式
[C:1]1(B(O)O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.Br[C:15]1[CH:20]=[CH:19][C:18]([C:21]([N:23]2[C:29]3[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=3[CH2:27][N:26]3[CH:34]=[CH:35][CH:36]=[C:25]3[CH2:24]2)=[O:22])=[C:17]([Cl:37])[CH:16]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1.C(O)C.O.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>[Cl:37][C:17]1[CH:16]=[C:15]([C:1]2[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[CH:4]=[CH:3][CH:2]=2)[CH:20]=[CH:19][C:18]=1[C:21]([N:23]1[C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][C:28]=2[CH2:27][N:26]2[CH:34]=[CH:35][CH:36]=[C:25]2[CH2:24]1)=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 10340Sodium CarbonateHCID 2545321-Naphthaleneboronic acidHCID 9909050HCID 9909050、化合物

生成物 1

HCID 21947737(2-Chloro-4-naphthalen-1-yl-phenyl)-(10,11-dihydro-5H-pyrrolo[2,1-c][1,4] benzodiazepin-10-yl)-methanone

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物触媒
HCID 702
Ethanol
溶媒
HCID 962Water溶媒
HCID 1140Toluene溶媒

実験手順

1-Naphthaleneboronic acid (0.52 g, 3.00 mmol) was added to a mixture of (4-bromo-2-chlorophenyl)-(5H, 11H-pyrrolo[2,1-c][1,4]benzodiazepin-10-yl)-methanone of Step A (1.27 g, 3.15 mmol) and sodium carbonate (0.53 g, 4.98 mmol) in toluene (22.5 mL), ethanol (4.5 mL) and water (9 mL). The resultant solution was purged with nitrogen for 10 minutes, then tetrakis(triphenylphosphine)palladium (0.18 g, 0.06 mmol) was added. The reaction mixture was heated to reflux for 76 hours. The solution was cooled to ambient temperature, then filtered through a pad of Celite, which was subsequently rinsed with ethyl acetate. The combined filtrate was diluted to 100 mL water/ethyl acetate (1:1). The aqueous layer was extracted with ethyl acetate, and the combined organic layer was dried over anhydrous magnesium sulfate, filtered, and evaporated to dryness to yield a brown oil. Purification by flash chromatography on silica gel eluting with hexane-ethyl acetate (5:1) resulted in a white solid which was dried under vacuum (0.62 g), m.p. 115–117.5° C.

後処理

  1. customThe resultant solution was purged with nitrogen for 10 minutes
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 76 hours
  4. filtrationfiltered through a pad of Celite, which
  5. washwas subsequently rinsed with ethyl acetate
  6. additionThe combined filtrate was diluted to 100 mL water/ethyl acetate (1:1)
  7. extractionThe aqueous layer was extracted with ethyl acetate
  8. dry with materialthe combined organic layer was dried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. customevaporated to dryness
  11. customto yield a brown oil
  12. customPurification by flash chromatography on silica gel eluting with hexane-ethyl acetate (5:1)
  13. customresulted in a white solid which
  14. customwas dried under vacuum (0.62 g), m.p. 115–117.5° C.

出典と根拠

ORDレコード
ord-7f7fd2463bc24e29a04ba1697dd80458
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07064120B2

反応ノート

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