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Cyanogen Bromide → HCID 178422405、化合物

HRID 1047311
ノート
印刷プレビュー

反応式

HRID 1047311 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([B:8]2[O:12][C:11]([CH3:14])([CH3:13])[C:10]([CH3:16])([CH3:15])[O:9]2)[CH:5]=[C:4]([NH2:17])[C:3]=1[NH2:18].[N:19]#[C:20]Br>CO>[CH3:1][C:2]1[C:3]2[NH:18][C:20]([NH2:19])=[N:17][C:4]=2[CH:5]=[C:6]([B:8]2[O:12][C:11]([CH3:14])([CH3:13])[C:10]([CH3:16])([CH3:15])[O:9]2)[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10476Cyanogen BromideHCID 666077053-Methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzene-1,2-diamine

生成物 1

HCID 178422405HCID 178422405、化合物収率 101.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-Methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzene-1,2-diamine (See Example 1.G) (500 mg, 2.015 mmol) and cyanic bromide (0.484 mL, 2.418 mmol) were added to a round bottom flask at room temperature, suspended in methanol (10.0 mL) and allowed to stir for 1.5 h. Volatiles were removed under reduced pressure followed by the addition of saturated sodium bicarbonate. The precipitate was collected via filtration, washed with ethyl acetate and dried under reduced pressure to afford the title compound (557 mg, 2.039 mmol, quant. yield). Compound was carried forward without further purification or characterization. MS (ESI) m/z 273.8 [M+1]+.

後処理

  1. customVolatiles were removed under reduced pressure
  2. additionfollowed by the addition of saturated sodium bicarbonate
  3. filtrationThe precipitate was collected via filtration
  4. washwashed with ethyl acetate
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-1faee54caa2748138d29fce6824b3410
出典データセット
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08569494B2

反応ノート

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