Triethylamine → 5-[Propyl-(4,5,6,7-tetrahydro-benzothiazol-6-yl)-amino]-pentanoic acid naphthalen-2-ylamide

HRID 1942395ノート

反応式

HRID 1942395 の反応式
[CH2:1]([NH:4][CH:5]1[CH2:13][CH2:12][C:8]2[N:9]=[CH:10][S:11][C:7]=2[CH2:6]1)[CH2:2][CH3:3].[CH:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][C:15]=1[NH:24][C:25](=[O:31])[CH2:26][CH2:27][CH2:28][CH2:29]Br.C(N(CC)CC)C>CC(C)=O>[CH:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][C:15]=1[NH:24][C:25](=[O:31])[CH2:26][CH2:27][CH2:28][CH2:29][N:4]([CH2:1][CH2:2][CH3:3])[CH:5]1[CH2:13][CH2:12][C:8]2[N:9]=[CH:10][S:11][C:7]=2[CH2:6]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 18705889Propyl-(4,5,6,7-tetrahydro-benzothiazol-6-yl)-amineHCID 669374455-Bromo-pentanoic acid naphthalen-2-ylamide

生成物 1

HCID 669374525-[Propyl-(4,5,6,7-tetrahydro-benzothiazol-6-yl)-amino]-pentanoic acid naphthalen-2-ylamide

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

9 is prepared from 1C and 9A using the same method as for 6 with acetone as solvent and triethylamine as base. Reaction temperature is 50° C. After evaporation of the solvent the residue is suspended in water, alkalized with sodium hydroxide solution and extracted three times with dichloromethane. After evaporation of the combined organic phases the product is crystallized as salt of maleic acid from acetonitrile/diethylether.

後処理

  1. customReaction temperature
  2. customis 50° C
  3. customAfter evaporation of the solvent the residue
  4. extractionextracted three times with dichloromethane
  5. customAfter evaporation of the combined organic phases the product
  6. customis crystallized as salt of maleic acid from acetonitrile/diethylether

出典と根拠

ORDレコード
ord-72f48c4767c14a9d8d616a8a90e2683e
出典データセット
uspto-grants-2013_03
特許番号
US08389555B2

反応ノート

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