Triethylamine → HCID 178458433, 화합물

HRID 2236742노트

반응식

HRID 2236742 반응식
Cl.[NH2:2][CH2:3][C:4]1[CH:5]=[CH:6][C:7]([O:11][CH2:12][CH2:13][CH3:14])=[C:8]([OH:10])[CH:9]=1.C(N(CC)CC)C.CO[CH:24]=[C:25]1[C:34]2[C:29](=[CH:30][CH:31]=[C:32]([N:35]3[CH:39]=[CH:38][CH:37]=[CH:36]3)[CH:33]=2)[C:28](=[O:40])[NH:27][C:26]1=[O:41]>CN(C)C=O>[OH:10][C:8]1[CH:9]=[C:4]([CH:5]=[CH:6][C:7]=1[O:11][CH2:12][CH2:13][CH3:14])[CH2:3][NH:2][CH:24]=[C:25]1[C:34]2[C:29](=[CH:30][CH:31]=[C:32]([N:35]3[CH:39]=[CH:38][CH:37]=[CH:36]3)[CH:33]=2)[C:28](=[O:40])[NH:27][C:26]1=[O:41]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 426258325-(Aminomethyl)-2-propoxyphenol hydrochlorideHCID 686931254-methoxymethylene-6-pyrrol-1-yl-4H-isoquinoline-1,3-dione

생성물 1

HCID 178458433HCID 178458433, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 5-aminomethyl-2-propoxy-phenol hydrochloride (109 mg, 0.50 mmole), 4 mL of N,N-dimethylformamide and triethylamine (75 μL, 0.54 mmole) is stirred for 15 minutes. Then (4-methoxymethylene-6-pyrrol-1-yl-4H-isoquinoline-1,3-dione (134 mg, 0.50 mmole) is added and the reaction mixture stirred for one hour. The reaction mixture is evaporated to dryness, taken up in 5% methanol in chloroform and passed through a short pad of Florisil eluting with 5% methanol in chloroform. The eluate is evaporated in vacuo and treated with acetonitrile, filtered and dried to give a beige solid, 94 mg, (45%), mp 215-216° C. dec; MS (ES+): m/z 418.2 (M+H).

후처리

  1. stirringthe reaction mixture stirred for one hour
  2. customThe reaction mixture is evaporated to dryness
  3. customThe eluate is evaporated in vacuo
  4. additiontreated with acetonitrile
  5. filtrationfiltered
  6. customdried
  7. customto give a beige solid, 94 mg, (45%), mp 215-216° C. dec

출처 및 근거

ORD 기록
ord-1002e16325fc4f38b7a7c03646426111
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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