Chloroform → HCID 20084584、化合物

HRID 1609283ノート

反応式

HRID 1609283 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:17](=[O:32])[C:18]1[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29](=[O:31])[CH3:30])=[CH:20][CH:19]=1)#[N:2].[BH4-].[Na+].C(Cl)(Cl)Cl>O1CCCC1.CO>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[NH:16][C:17](=[O:32])[C:18]1[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH2:26][CH2:27][CH2:28][CH:29]([OH:31])[CH3:30])=[CH:22][CH:23]=1)#[N:2]

参加物

6

反応物 3

HCID 6212ChloroformHCID 4311764Sodium borohydrideHCID 20084436HCID 20084436、化合物

生成物 1

HCID 20084584HCID 20084584、化合物収率 94.2%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In 30 ml of tetrahydrofuran was suspended 3.33 g of N-[2-(2-cyanophenylthio)phenyl]-4-(5-oxohexyloxy)benz-amide (prepared in accordance with Reference Example 6, Step 2) followed by addition of a solution of 0.31 g of sodium borohydride in methanol, and the mixture was stirred for 1 hour. To the reaction mixture was added chloroform and the mixture was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethyl acetate-n-hexane to give 3.15 g of the title compound as white crystals.

後処理

  1. washthe mixture was washed with saturated aqueous sodium chloride solution
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-e5124195e9134832b1331333fe0b7e28
出典データセット
uspto-grants-1995_03
特許番号
US05399703

反応ノート

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