홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1,2-Dichloro-4-isothiocyanatobenzene → HCID 178462557, 화합물

HRID 2371130
노트
인쇄 미리보기

반응식

HRID 2371130 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]=[C:10]=S)[CH:5]=[CH:6][C:7]=1[Cl:8].[N:12]#[C:13][NH2:14].[Na].Cl.CN(C)CCCN=C=NCC.[CH2:28]([N:30]1[CH2:35][CH2:34][CH2:33][C@@H:32]([CH2:36][N:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH2:31]1)[CH3:29]>C(O)C.CN(C)C=O>[C:13]([N:14]=[C:10]([N:40]1[CH2:39][CH2:38][N:37]([CH2:36][C@@H:32]2[CH2:33][CH2:34][CH2:35][N:30]([CH2:28][CH3:29])[CH2:31]2)[CH2:42][CH2:41]1)[NH:9][C:4]1[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=1)#[N:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 230651,2-Dichloro-4-isothiocyanatobenzeneHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 57375518CyanamidnatriumHCID 576568471-{[(3R)-1-ethylpiperidin-3-yl]methyl}piperazine

생성물 1

HCID 178462557HCID 178462557, 화합물수율 37.6%

시약·촉매·용매 2

HCID 702
Ethanol
용매
HCID 6228Dimethylformamide용매

실험 절차

3,4-Dichlorophenylisothiocyanate (204 mg) and sodium hydrogen cyanamide (70 mg) were refluxed in ethanol (20 ml) for three hours. The mixture was allowed to cool to room temperature then 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (211 mg), 1-{[(3R)-1-ethylpiperidin-3-yl]methyl}piperazine (220 mg) and N,N-dimethylformamide (2 ml) were added and the reaction left to stir for 18 hours then concentrated in vacuo. The crude product was subjected to reverse phase HPLC using a gradient of 95% water/acetonitrile/0.1% TFA through to 50% water/acetonitrile/0.1% TFA. The combined product fractions were concentrated in vacuo then separated between dichloromethane (50 ml) and saturated sodium bicarbonate solution (100 ml). The dichloromethane layer was separated, dried over magnesium sulphate, filtered and concentrated in vacuo to give the title compound (159 mg).

후처리

  1. waitthe reaction left
  2. concentrationthen concentrated in vacuo
  3. concentrationThe combined product fractions were concentrated in vacuo
  4. customthen separated between dichloromethane (50 ml) and saturated sodium bicarbonate solution (100 ml)
  5. customThe dichloromethane layer was separated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a4bb133355e14354811bdf93fc91db2a
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08710224B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트