Water → Methyl [4-cyano-1-(trifluoroacetyl)-2,3-dihydro-1h-1-benzazepin-2-yl]acetate

HRID 1761028

反応式

HRID 1761028 の反応式
[F:1][C:2]([F:30])([F:29])[C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH:9]=[C:8](OS(C(F)(F)F)(=O)=O)[CH2:7][CH:6]1[CH2:24][C:25]([O:27][CH3:28])=[O:26])=[O:4].[Li][C:32]#[N:33].C1OCCOCCOCCOC1.O>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:32]([C:8]1[CH2:7][CH:6]([CH2:24][C:25]([O:27][CH3:28])=[O:26])[N:5]([C:3](=[O:4])[C:2]([F:29])([F:1])[F:30])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH:9]=1)#[N:33]

参加物

7

反応物 4

HCID 962WaterHCID 92691,4,7,10-TetraoxacyclododecaneHCID 91577583Methyl (1-(trifluoroacetyl)-4-{[(trifluoromethyl)sulphonyl]oxy}-2,3-dihydro-1h-1-benzazepin-2-yl)acetateHCID 178506913HCID 178506913、化合物

生成物 1

HCID 91539061Methyl [4-cyano-1-(trifluoroacetyl)-2,3-dihydro-1h-1-benzazepin-2-yl]acetate

試薬・触媒・溶媒 2

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

実験手順

A solution of the compound obtained in Step e (1.35 g; 293 mmol) in 16 ml of anhydrous toluene is added to a mixture of LiCN (0.5 M in DMF) (11.72 ml; 5.86 mmol), (Ph3P)4Pd (237 mg; 0.205 mmol) and 12-crown-4 (36 mg; 0.205 mmol) under an argon. atmosphere. The reaction mixture is stirred at ambient temperature for 6 hours. Water (10 ml) is added to the reaction mixture, and the organic phase is extracted with diethyl ether. After drying and concentration, the residue obtained is purified on silica gel (eluant:heptane/EtOAc) to yield the title product.

後処理

  1. extractionthe organic phase is extracted with diethyl ether
  2. customAfter drying
  3. concentrationconcentration
  4. customthe residue obtained
  5. customis purified on silica gel (eluant:heptane/EtOAc)

出典と根拠

ORDレコード
ord-509b45decb944185882a990907552a84
出典データセット
uspto-grants-2005_01
特許番号
US06846833B2

関連ノート

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