Methanol → 10,11-Dihydrodibenzo(b,f)(1,4)thiazepine

HRID 962503ノート

反応式

HRID 962503 の反応式
O=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][CH:15]=[CH:16][C:4]=2[NH:3]1.B.CSC.CO>O1CCCC1>[CH:9]1[C:8]2[CH2:2][NH:3][C:4]3[CH:16]=[CH:15][CH:14]=[CH:13][C:5]=3[S:6][C:7]=2[CH:12]=[CH:11][CH:10]=1

参加物

5

反応物 3

HCID 887MethanolHCID 374829DibenzothiazepinoneHCID 12423031(Dimethyl sulfide)trihydroboron

生成物 1

HCID 1231048210,11-Dihydrodibenzo(b,f)(1,4)thiazepine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a mixture of 3.3 g of 10,11-dihydro-11-oxodibenz[b,f] [1,4]thiazepine in 25 ml of tetrahydrofuran is added 4.0 ml of 10 molar borane-dimethylsulfide in tetrahydrofuran. The mixture is stirred at room temperature for 18 hours, 50 ml of anhydrous methanol added and the solvent removed. An additional 30 ml of methanol is added and the solvent removed to give white crystals. A sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent to give white crystals, m.p. 145°-148° C.

後処理

  1. customthe solvent removed
  2. additionAn additional 30 ml of methanol is added
  3. customthe solvent removed
  4. customto give white crystals
  5. customA sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent
  6. customto give white crystals, m.p. 145°-148° C.

出典と根拠

ORDレコード
ord-0d2ca8e5867c4fff846e7e5a15043659
出典データセット
uspto-grants-1998_06
特許番号
US05760031

反応ノート

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