Diisopropylethylamine → HCID 178473956, 화합물

HRID 858300노트

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HRID 858300 반응식
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[CH2:6][C:5]1=[O:14])(=[O:3])[CH3:2].[CH3:15][N:16]1[C:20]2[CH:21]=[CH:22][C:23]([C:25](O)=[O:26])=[CH:24][C:19]=2[N:18]=[CH:17]1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C(N(C(C)C)C(C)C)C>CN(C=O)C.O>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:13])[CH:11]=2)[C:6](=[C:25]([OH:26])[C:23]2[CH:22]=[CH:21][C:20]3[N:16]([CH3:15])[CH:17]=[N:18][C:19]=3[CH:24]=2)[C:5]1=[O:14])(=[O:3])[CH3:2]

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 49130631-Methyl-1H-benzimidazole-5-carboxylic acidHCID 116441611-Acetyl-6-chloroindolin-2-one

생성물 1

HCID 178473956HCID 178473956, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

3.5 g of 1-acetyl-6-chloro-2-indolinone, 3.4 g of 1-methylbenzimidazole-5-carboxylic acid, 6.1 g of TBTU, 2.9 g of HOBT-hydrate and 8.7 ml ethyldiisopropylamine are stirred in 100 ml DMF for 15 hours at ambient temperature. The mixture is combined with water and extracted with ethyl acetate, while the crude product is partially precipitated. The residue obtained by distilling off the solvent is taken up in dichloromethane and a little methanol and extracted with water. The organic phase is evaporated down, the residue stirred successively with ethyl acetate and diethyl ether, suction filtered and dried.

후처리

  1. extractionextracted with ethyl acetate, while the crude product
  2. customis partially precipitated
  3. customThe residue obtained
  4. distillationby distilling off the solvent
  5. extractiona little methanol and extracted with water
  6. customThe organic phase is evaporated down
  7. filtrationfiltered
  8. customdried

출처 및 근거

ORD 기록
ord-7edb584066814722a69e407c4a7261c6
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07148249B2

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