Cyanogen Bromide → HCID 69373404, 화합물

HRID 1372474노트

반응식

HRID 1372474 반응식
[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

참가 물질

5

반응물 3

HCID 10476Cyanogen BromideHCID 14923Ammonium HydroxideHCID 6157743-Iodobenzohydrazide2회

생성물 1

HCID 69373404HCID 69373404, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5eb302d548784ab4b320fcfecb51b6d9
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157490B2

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