Cyanogen Bromide → HCID 69373404、化合物

HRID 1372474ノート

反応式

HRID 1372474 の反応式
[N:1]#[C:2]Br.[I:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][CH:14]=1)[C:8]([NH:10]N)=[O:9].[OH-].[NH4+:16]>CO>[NH2:16][N:1]1[CH2:2][N:10]=[C:8]([C:7]2[CH:12]=[CH:13][CH:14]=[C:5]([I:4])[CH:6]=2)[O:9]1

参加物

5

反応物 3

HCID 10476Cyanogen BromideHCID 14923Ammonium HydroxideHCID 6157743-Iodobenzohydrazide2 回

生成物 1

HCID 69373404HCID 69373404、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of cyanogen bromide (1.06 g, 10.0 mmol) in 10 mL of methanol was added dropwise to an ice-cold suspension of 3-iodobenzhydrazide (2.62 g, 10.0 mmol, Intermediate 7, Step A) in 20 mL of methanol. After 30 min, the mixture was allowed to warm to room temperature and was then warmed at reflux for 1.5 h. The resultant solution was cooled to 0° C., and neutralized to pH 9 with concentrated aqueous ammonium hydroxide. The resultant precipitate was collected, washed with methanol, and dried in vacuo to afford the product as an off-white powder. LC/MS 288.0 (M+1).

後処理

  1. temperaturewas then warmed
  2. temperatureat reflux for 1.5 h
  3. customThe resultant precipitate was collected
  4. washwashed with methanol
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-5eb302d548784ab4b320fcfecb51b6d9
出典データセット
uspto-grants-2007_01
特許番号
US07157490B2

反応ノート

読み込み中…