1-Hydroxybenzotriazole → HCID 131731158、化合物

HRID 926426ノート

反応式

HRID 926426 の反応式
[NH:1](C(OCC1C2C(=CC=CC=2)C2C1=CC=CC=2)=O)[C@H:2]([C:4]([NH:6][CH2:7][C:8]([OH:10])=O)=[O:5])C.[NH2:28][C@H:29]([CH:37]=[O:38])[CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[CH3:39]N(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1.C(N(C(C)C)CC)(C)C>CN(C)C=O.ClCCl>[NH2:28][C@H:29]([C:37]([NH:1][CH2:2][C:4]([NH:6][C@H:7]([CH:8]=[O:10])[CH3:39])=[O:5])=[O:38])[CH2:30][C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1

参加物

8

反応物 5

HCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 446207HCID 446207、化合物HCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 7019065HCID 7019065、化合物2 回

生成物 1

HCID 131731158HCID 131731158、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

(Phe)-H was synthesized by the solid phase reaction method using CTC as a solid phase carrier. Furthermore, similar to Example 7, Fmoc-Ala-Gly-OH was synthesized. Then, to dichloromethane (2 ml) were added CTC-Phe-H (110 mg (0.145 mmol)), Fmoc-Ala-Gly-OH (160 mg (0.4 mmol)), HBTU (165 mg (0.4 mmol)), HOBt (60 mg (0.4 mmol)), dimethylformamide (1 ml) and diisopropylethylamine (75 μl (0.4 mmol)), respectively, and the mixture was stirred to react at room temperature for 2 hours. After the reaction, the solid phase was washed with dimethylformamide (3×2 ml), methanol (3×2 ml) and dichloromethane (3×2 ml), respectively. Subsequently, to the above solid phase was added the previously prepared Fmoc deprotection solution (dimethylformamide:piperidine:DBU=96:2:2) (2 ml), and the mixture was stirred to react at room temperature for 1 hour to obtain CTC-Phe-Gly-Ala-H.

後処理

  1. customto react at room temperature for 2 hours
  2. customAfter the reaction
  3. washthe solid phase was washed with dimethylformamide (3×2 ml), methanol (3×2 ml) and dichloromethane (3×2 ml)
  4. additionSubsequently, to the above solid phase was added the previously prepared Fmoc deprotection solution (dimethylformamide:piperidine:DBU=96:2:2) (2 ml)
  5. stirringthe mixture was stirred
  6. customto react at room temperature for 1 hour

出典と根拠

ORDレコード
ord-82be9c9f477243a2a46c93dbe4aed6bd
出典データセット
uspto-grants-2016_03
特許番号
US09284348B2

反応ノート

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