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Hydrochloric Acid → Methyl 3-oxo-2,3-dihydro-1-benzoxepin-7-carboxylate

HRID 1791040
ノート
印刷プレビュー

反応式

HRID 1791040 の反応式
N12CCCN=C1CCCCC2.[O:12]=[C:13]1[CH2:19][CH:18](S(C2C=CC=CC=2)(=O)=O)[C:17]2[CH:29]=[C:30]([C:33]([O:35][CH3:36])=[O:34])[CH:31]=[CH:32][C:16]=2[O:15][CH2:14]1.O.Cl>ClCCl>[O:12]=[C:13]1[CH:19]=[CH:18][C:17]2[CH:29]=[C:30]([C:33]([O:35][CH3:36])=[O:34])[CH:31]=[CH:32][C:16]=2[O:15][CH2:14]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 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 22042264Methyl 3-oxo-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate

生成物 1

HCID 11138567Methyl 3-oxo-2,3-dihydro-1-benzoxepin-7-carboxylate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

0.084 ml (1.05 equivalents) of 1,8-diazabicyclo[5.4.0]undec-7-ene is added at ambient temperature to 217 mg (0.6 mmol) of methyl 3-oxo-5-(phenylsulfonyl)-2,3,4,5-tetrahydro-1-benzoxepin-7-carboxylate, prepared according to example 2, in suspension in 20 ml of dichloromethane. From the addition of the base, the medium becomes translucent and slightly yellow. After addition of water and 1N hydrochloric acid, the phases are separated by settling and then the aqueous phase is extracted three times with dichloromethane. The combined organic phases are washed with a saturated sodium hydrogencarbonate solution and then with brine. After drying and then concentrating under vacuum, 90 mg (68%) of methyl 3-oxo-2,3-dihydro-1-benzoxepin-7-carboxylate are obtained in the form of a white solid; M.p.=89–93° C.

後処理

  1. customprepared
  2. additionFrom the addition of the base
  3. customthe phases are separated
  4. extractionthe aqueous phase is extracted three times with dichloromethane
  5. washThe combined organic phases are washed with a saturated sodium hydrogencarbonate solution
  6. customAfter drying
  7. concentrationconcentrating under vacuum, 90 mg (68%) of methyl 3-oxo-2,3-dihydro-1-benzoxepin-7-carboxylate
  8. customare obtained in the form of a white solid

出典と根拠

ORDレコード
ord-eb8285bcd2b84ff3b1be95b859facf7a
出典データセット
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07071340B2

反応ノート

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